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	BrightStar (Moderator) 06-30-00 12:45 No 23351		Post deleted by LaBTop	Bookmark Reply
	LaBTop (Stranger) 06-30-00 15:18 No 23406		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			Poster: LaBTop Subject: Re: Detailed Methods for Non-chemists . P2P--> METHAMPHETAMINE, racemic mix. : --------------------------------------------------------------------------- Materials : See MDMA, Isosafrole etc. --------------------------------------------------------------------------- Chemicals : See MDMA, exept : Change MDP2P to P2P, Phenyl-2-propanone. Method : THIS IS THE MAIN PROCEDURE FOR ALL ONE POT xxBORO/xxxP2P/xxxAMINE SYNTHESES !!!! The original link is broken, or the file is deleted, so: LaBTop .......... posted 06-23-99 01:04 PM Member Making of d,l-Meth (Ice). Ingredients: • 138 gram P2P = +/- 1 grammole. • 1000 ml Methanol (+ 10 % weight Methylaminegas dissolved in it = +/- 100 gram)= +/-3gmol. • 36 gram MgSO4.7H2O , magnesiumsulfate (dry at 300 C for 2 Hrs in oven to get MgSO4.zeroH2O)= to dry Methanol/M.A. mix . • 200 ml Silicagel balls +/- 3 to 5 mm (dry at 300 C for 2 Hrs in oven, changes to dark brown! ),=to attrack 2 gmol H2O, during imine forming. • 15 gram NaBH4 as a reducing agent for the formed (waterfree !) Imine. IMPORTANT: THE REACTION IS VERY SENSIBLE FOR ANY WATER (fluid or vapour in the air!). First quickly crunch your pre-dried (oven, 300 C, 3 hrs.)DRY MgSO4 to pop corn shaped rocks in a mortar, sieve the powder out, and directly put only the rocky, dry MgSO4 under max. mixing in the Methanol/Methylamine mix and close the pot, to let NO water from the air in. Keep mixing for 10 minutes, then all the water will be taken up to the MgSO4. Let stand and wait till all the MgSO4 is on the bottom. Now quickly tap off the now DRY MeOH/MA mix in a 2L reaction flask and close that one. (Wash directly your wet empty pot with lots of water, to remove the smell of methylamine so you can safely dry and store it back in the cupboard). Now add the 200 ml (measure in beaker, neglect the free spaces) DRY Merck or other brand, Silicagel beads (2-5 mm) and a magnetic mixer bar also in the 2L flask and close again. Keep 2L flask in Silicone-oil bath at 20 C. Do not use heater switch! Silicone-oil only slowly warms up, so can absorp lots of heat! Do not apply heat now, it's only meant as a cooling medium in this stage, to keep the temperature from the liquids at nearly the same value. Now add SLOWLY via a dropping funnel the 138 gr P2P to the 2L flask under strong mixing. The temperature rises to 23 C during the (waterfreed) Imine forming. The water formed in this reaction is taken up by the dried Silicagel! This takes 30 minutes. Let then mix for another 1 hour. The reactionmix color changes from light yellow to coffee+milk color. End Temperature = 23 C. So it is an exothermic reaction, it releases heat. Stop mixing after this 1 hour and pour the fluid off into a 2L glas erlenmeyer with flat bottom and add a mixbar. The remaining Silicagel is washed 3 times with 50 ml DRIED (use silicagel) methanol, to catch the remaining Imine, and those 2 x 50 ml is also poured into the 2L erlenmeyer. Now put the 2L erlenmeier on a magn.mixer, in an icecube's (no water!)/methanol bath (-10 C) and start strong mixing. Put a Funnel on top of 2L erlenmeier, in rubber ring. Now start adding, every 5 min., a teaspoonfull (flat off!) of boro and wash in with minimum methanol. After every spoonfull, stopper the funnel loosely with a rubber stopper. This takes 2,5 hrs. DO NOT exceed a temp of more then 20 C !! You can add the next spoon at +/-8 C. Solution color is light clear orange/brown. Let mix in total for 8,5 hrs.(could perhaps be lot less hours, do'nt want to know: time is NOT money!) The total volume is +/- 1900 ml. Add then the total volume mix to 5 L dest. water in a 10 L flask, under magn.mixing. The pH=12 . Add then 500 ml DiChloroMethane (DCM) and mix strongly for 30 min. Let oil precipitate and a dark, honey-coloured layer of DCM+oil is on the bottom. Suck the waterpart carefully off with an aspirator + siliconetube. Fill the rest (little water+DCM+freebase-oil) in a seperator funnel and tap off only the DCM+oil = 550 ml. The leftover MgSO4 and boro salts stayed nicely in the waterpart. Then dry the DCM+oil with some DRY MgSO4 and decant in 2L erlenmeier. Wash this MgSO4 with some fresh, DRY DCM and add the DCM washings to the now dry DCM+oil. Total volume DCM+oil = 1000 ml, colour is honey/red. Start now bubbling this 1000 ml with DRY HCl-gas, while 2L erlenmeier stands in icebath on magn.mixer and mix fairly strong. Check pH frequently, proceed until pH 6. Crystals will not form, that comes now. Pour the now acidified 1000 ml in a 2 L evap.flask and put on digital Heidolph Rotavap machine. Speed= 100 rpm , temp= 80 C, mode= p/auto, (little)vacuum= 800 mbar, (to hold the flask). After distillating off nearly all the DCM (DCM boiling point=40 C), suddenly the contents of the flask turns from dark honey colour to creamy milk color and it dries out to a round cake on the bottom. Remove the 1 L DCM, evapped into the collector flask, and hang that empty flask on again. Now put full vacuum on (less than 20 mbar) to remove the last traces of water. Cleaning by 1 time recrystalization: Put MINIMUM quantity of hot (40 C) DRY DCM (or dry 98+% Ethanol) in the flask with the dry cake, until the last remains of the dry cake dissolve, and add 4 x this DCM-quantity in the form of DRY acetone. Close with stopper, swirl a few times around and put 1 hr (or more, if needed)in freezer. A solid dirty-white crystal mass is formed with a layer of dark red fluid on top of it. Decant the red DCM fluid, evaporate the last DCM off with aspirator vacuum and wash wet crystals 3 to 4 times with dry acetone. You have, the last time, snow white crystals. Dry Weight = 141,5 gram, close to quantitative yield. You can eventually melt this crystal mass in an alu flatbottom pot on a heaterplate at 170-175 C. Then let this melt, VERY SLOWLY, and do not go higher then necessary to melt it, or its starts smoking ( you have your first quick-test then: enjoy!). Cool down to 150 C again, really slowly, 1 degree C per 30 min. (regulate with your temp controller!), and you got d,l-ICE, after you let it very slowly again cool down to roomtemperature (with a closed lid on it!, its hygroscopic ! ). Advantage: you removed ALL the water in this process!!! You can better make the sulfate salt following Logicals method : Let 10% H2SO4/Ethanol mix acidify a 1:4 mix of freebase Meth/Ethanol. This salt is not so hygroscopic. Filter and dry the crystals. So now you know at last how to make ICE cream... Ravers LOVE it!!!! LT/ --------EMOTIONSwill always beFREE!-------- LaBTop posted 06-23-99 01:19 PM Member Yohoo, forgot to tell:Use d-Tartraric acid to get d-Meth !!!!!!!! 2 Flies in one hit.... Ask your beloved moderator, the unforgettable Mr. Spit_tartrar_Ball, he knows how to do that, he recently posted the method, but needs a little explaining for most of you, I'm afraid. But thou should NOT be afraid, its easy! He only made a serious error then, see explanation how to make d-Methamphetamine from racemic mixed Methamphetamine in the "Chirality of MDMA" post, further on down in this thread. Then you have d-Meth (the softer part) AND l-Meth (which is speedy only). Life becomes easier and easier......? LT/ ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ Sunlight's method of preparing 10% Methylamine solution in Methanol, from aequous 40% Methylamine. This is a convenient adaptation of the NaBH4 One Pot procedures using aqueous Methylamine instead of the gaseous form. He liberated the MeNH2 as a gas with dry NaOH pellets : sunlight (Hive Researcher)07-10-00 02:15 If you should try to use directly a 40% aq. MeNH2 solution you will get a 60 % yield based on the pure ketone. The procedure to dehydrate ( get rid of the water-part) the aq. methylamine is, for example: Put in a 2-neck flask 700 grams of commercial dry NaOH, and using a compensating pressure separatory funel attached to one of the necks, add slowly over one hour 350 cc of aq. methylamine to the NaOH. In the other neck attach a rubber stopper with a teflon tube and to it a glass tube with a gas diffusor ( a tiny glasfunnel with a glasfilter glued in it with 6 seconds glue or two component glue or just melt it tight with a torch ), and bubble the MA-gas in 1000 cc of methanol in a flask in a methanol- or water/ice bath. Reaction is endothermic, so it cools down, finally you can heat a bit the NaOH containing flask to force the liberation of the last gas, but it's not really necessary, just shake it to see a homogeneus paste. The compensation of pressure can be done using a regular separatory funel if you attach a 1-hole rubber stopper with a teflon tube connecting to the NaOH flask, if you use a 3-neck flask you can use the other neck, and if you use a two neck flask, you can use in one of the necks a 2-hole rubber stopper, 1 hole connecting to the stopper in the neck of the separatory funnel and one to the ... dripping hole of it (sorry, it's my english...). You can refill your sep. funnel with aq. methylamine if it's not enough big to complete the whole liberation of all the gas, close the valve and close the other tube, open it and put the aq. solution in, then stop it and free the other tube. The absortion of methylamine in methanol at 0-5 C is perfect, you don't even need to redirect possible fumes from the methanol, there aren't, but stop the flask with some papertissue to prevent the entry of humidity. The gas diffusor can be done with a regular glass tube, try to enlarge a bit one of the ends, and then try to weld inside it a piece of fine filterglass for the gas bubbles feed, it will act as a diffusor, not very good, but enough, and it won't heighten the pressure too much (one stopper could jump and you would have a toxic ambient atmosphere of methylamine in your viginity). Probably using a pipette will work, absortion is very good. You can weight finally the 10% methanolic solution of methylamine to know the exact weight of gas you have in it (you weighted it before). You will have a bit of water, but don't worry, mix it with the ketone (350 grams), add silica gel (160 gr) and shake and let stand , shake and so on ... during an hour, filter and wash the silica with 200 - 300 cc of methanol, add the NaBH4 at +7 C ( an ice/salt bath works fine) to get from 75 - 87 % of the desired product, depending on the purity of your ketone. You can dehydrate the methylamine gas by passing it through a flask with NaOH, but it's not necessary due to the addition of silica gel.   Beaker (Hive Researcher)07-10-00 10:11  From http://rhodium.lycaeum.org/chemistry/meam-pdc.txt  : " KrZ (Hive Researcher) : The mix {MeNH2 + 2H2O (The product of catalytic hydrogenation of methylamine) in methanol with Na2SO4} was split in half and each half sat with 1500g of Na2SO4 for an hour, with occasional stirring. The Na2SO4 ( sodiumsulfate) was filtered off for a long time, until it was quite dry in appearance, the mix halves were combined and washed 2x with 1L of CH3OH (methanol), which was filtered off and added back to the solution." sunlight (Hive Researcher) 07-11-00 00:39  We did something similar with MgSO4, trying to dry a mixture of 40% MeNH2 and methanol, and the end product was titrated and it was about 3 % instead of 10 % w/w (weight/weight), the MgSO4 had a strong smell of methylamine, so we thought most of the gas was ended in the water and in the magnesiumsulfate, and we tried the above procedure, that works fine. ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ IVa.--- 2,5-DIMETHOXYBENZALDEHYDE---> 2CH---> 2CB Consult for more details this thread : Post No 26600 Posted by :   Beaker (Hive Researcher) 07-09-00 00:48 2CB for the LAH impaired. The following is a synthesis of 2CB from 2,5-dimethoxybenzaldehyde that does not require the use of the slightly hazardous and/or difficult to obtain reagents normally associated with its synthesis, notably LAH, pressurized H2, and Br2. No doubt some clandestine chemists have been discouraged from attempting the synthesis of what is, IMHO, a pretty cool substance by the nature of these reagents and the lack of a clearly written procedure for an alternate route that does not use them. However, alternate routes do exist, and one of them is detailed below. Note that this route does require one additional step to acheive the nitrostrene reduction than with the use of H2 or LAH, but that the yield is actually substantially higher than what others have reported with those reducing systems. Also, the bromination procedure is somewhat unrefined at present and does not result in the greatest of yields or the easiest of workups, so feel free to use the classical procedure if you want to make or buy your own bromine. As a final note, although this route will happily accomodate batch sizes of ~50g in 2L glassware, it does not scale anywhere near as well as catalytic hydrogenation, so if you're trying to go huge, it's probably not for you.Scaleup should not be a problem, but due to the rather low product loading that you can obtain with the method as written, it is rather impractical at >50g scale. Bigger than that and I would suggest that one look into catalytic hydrogenation a la KrZ's mescaline writeup or finding a way to cut the amount of solvent back quite a bit. For most people, ~80g of 2CB out of 100g, or $60 worth of 2,5-dimethoxybenzaldehyde is more than enough. Step 1 Condensation of 2,5-dimethoxybenzaldehyde with nitromethane In a 500mL RBF equipped with a relfux condensor and a stir bar, place 100g 2,5-dimethoxybenzaldehyde, 15g ammonium acetate, and 250mL of nitromethane. Heat to a gentle reflux while magnetically stirring. Maintain reflux for ~45min, by which time the color of the solution should progress from clear/yellow to a deep reddish-black. Remove heat and carefully pour the hot rxn mixture into 1L of ice-cold 70% IPA. Allow the IPA/rxn mixture to stand for a while. You should now have a flask full of orange solids floating in red/black mother liquor. Vacuum-filter the solids and wash them with additional portions of ice-cold 70% IPA until the filtrate is no longer reddish(It will become very slightly orange in color with small amounts of dissolved nitrostyrene). Thoroughly dry the collected orange solids by pulling air through the filter for a while and then dry under vaccum. It is very important that the nitrostyrene be completely dry before proceding to the next step. Yield - 106.1g (84%) of 2,5-dimethoxynitrostyrene Purity - Single spot by TLC, NMR is clean. Step 2 Sodium borohydride reduction of 2,5-dimethoxynitrostyrene Into a dry 2L RBF flask equipped with a stir bar was added 400mL of anhydrous ethanol(If you can't get anhydrous ethanol, use anhydrous IPA. DO NOT USE METHANOL!!!). The rxn was cooled to 0C in an ice/water bath and 36.2g of sodium borohydride was added(slight H2 evolution). A pressure-equalized addition funnel was charged with a pre-made saturated solution of 50g 2,5-dimethoxynitrostyrene in THF(about 600mL) and attached to the flask. A piece of tubing was attached to the top of the addition funnel and run outside to vent the hydrogen that will evolve during the course of the reaction. While maintaining the ice/water bath, all of the bright yellow nitrostyrene solution(refill the addition funnel if necessary) was slowly(reaction is exothermic, so watch it) added to the sodium borohydride solution over the course of ~90 min (Note: gas will evolve over the course of the addition. It is H2. Be careful). After the addition is complete, the rxn was allowed to stir for an additional 10 min and then poured into a 4L erlenmeyer containing 1L of H2O and a 3" stir bar (H2 evolution). While stirring, 250mL GAA (Heavy H2 evolution) was carefully added (one could use 400 mL 31.45% HCl). The quenched reaction mixture was divided into three portions. In a 2L sep funnel, each portion was combined with 500mL Et2O(or toluene) and 500mL brine. The funnel was shaken and the aqueous (bottom) layer was discarded. The organics were washed with 3 additional 500mL portions of brine (conc. NaCl sol.). This was repeated with the other two portions. The organics were combined, dried over MgSO4, filtered and the solvent evaporated to give a clear yellow oil. Yield - 47.0g of crude 2,5-dimethoxynitroethane. Purity - Two spots by TLC. NMR analysis indicates a 50:1 molar ratio of the desired product to dimeric impurity(this is the only impurity present). Adjusted yield of 2,5-dimethoxynitroethane is 45.2g (89.5%). Step 3 Catalytic Transfer Hydrogenation of Crude 2,5-dimethoxynitroethane The crude product of the previous step was dissolved in 400mL MeOH and placed in a 1L RBF equipped with a stir bar. In a separate beaker away from all combustible materials, 1g of 10% Pd/C was carefully wetted down with MeOH and the resulting slurry transferred to the rxn flask. To the rxn flask was added 62g ammonium formate. The flask was equipped with a reflux condensor, a piece of tubing was attached to the top of the condensor, and the end of the tubing was submenged in a container of water (this works to exclude O2 from the rxn while allowing the evolving CO2 to escape). The rxn was gently refluxed for 24 hr.(CO2 evolution), cooled, filtered through celite to remove the Pd/C, and the solvent evaporated. The residue was taken up in 150 mL of Et2O (or toluene) and 300 mL of H2O and the pH adjusted to >12 with 20% NaOH. The mixture was transfered to a sep funnel, shaken, and separated. The aqueous layer was extracted with 2 x 100 mL portions of Et2O (or toluene). The combined organics were dried over MgSO4, filtered, and gassed with HCl (2CH x HCl is partially soluble in DCM, so don't gas in that solvent). The resulting white crystalline solids were filtered, washed with Et2O, and allowed to air dry to give 2CH Hydrochloride. Yield - 43.8g (94%) of 2CH Hydrochloride. Purity - Single spot by TLC. NMR is clean. Step 4 Bromination of 2CH Freebase The 2CH x HCl was dissolved in a 300 mL H20. The pH was adjusted to >12 with 20% NaOH and the aqueous layer was extracted with 4 x 100 mL DCM. The DCM was evaporated to give 2CH freebase, which was dissolved in 500 mL of 3:1 AcOH/H2O. The rxn was cooled to 0C in an ice/water bath. 37.3g of 48% aq. HBr was added, followed immediately by 23.8g of 30% H2O2. The rxn was stirred for 6 hr, allowing the ice bath to melt. The majority of the AcOH was removed under vacuum and the nasty reddish-black rxn mixture was partitioned between 1L H20 and 500 mL EtOAc(EtOAc was found to be much better for dissolving the impurities in this rxn than Et2O or toluene. This is messy at first, but everything should go into solution after much agitation). The layers were separated and the aqueous extracted with an additional 500 mL EtOAc. The aqueous was basified to pH >12 with 20% NaOH and extracted with 3 x 200 mL portions of Et2O. The combined organics were washed with 400 mL brine, dried over MgSO4, filtered and gassed with HCl. The resulting tan crystalline solids were filtered and recrystalized from boiling 1:1 IPA/Toluene to give pure 2CB x HCl as a white crystaline solid. Yield - 34.0g (57%) of 2CB Hydrochloride. Purity - Single spot by TLC. NMR is clean. I have references for the two reduction steps and the bromination, but can't seem to find them. If someone asks really nicely I might be persuaded to find and post them. Also, before some jackass reads this procedure and asks me why 4 eq.of sodium borohydride is used for the reduction, here is a interesting little table for your reading pleasure. (Eq. NaBH4) -> Molar ratio of 2,5-dimethoxynitroethane to dimer. (2.5) -> 6.25 : 1 (3.5) -> 44 : 1 (4.0) -> 50 : 1      Rhodium (Chief Bee) 07-09-00 05:55  Beaker - this was certainly one of the single best posts to the Hive after the software change! Great!  ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ 2C-B Synthesis a la Lycaeum. 4-Bromo-2,5-dimethoxyphenethylamine ____________________________________________________________ List of Chemicals :  100g 2,5-Dimethoxybenzaldehyde  10g Ammonium acetate  200g Nitromethane  Isopropyl Alchohol (IPA)  500ml Tetrahydrofuran (THF)  Anhydrous Calcium Chloride (eg, Drierite)  NaOH  HCl  20 gram Bromine  Glacial acetic acid  Methylene chloride  25 grams of LAH ____________________________________________________________ List of Materials :  500ml boiling flask  200ml boiling flask  condenser  electric heater/heating mantel  oil bath  boiling chips  filter paper  separation funnel  high-temperature distillation flask  250ml filter flask  2 250ml beakers  500ml beaker  vacuum pump and hose  thermometer ____________________________________________________________ DISCLAIMER #1: It should be perfectly clear that 2-CB, also known under a variety of names such as "venus", "bromo", "erox", or "nexus", is currently a Schedule-I substance. In order to protect us from ourselves, our government has dutifully made it illegal to posses, manufacture, or distribute any amount of 2-CB for any purpose. Any persons caught breaking this law are subject to prosecution, imprisonment, dehumanization, demonization, humiliation, character defamation, intense personal harrasment, and to top it all off - drug diversion. You've been warned. DISCLAIMER #2: It should be made perfectly clear that laboratory chemistry is a very unforgiving art form. It can take years to master even the simplest of reactions and tiny mistakes can literally blow up in your face. Although this synthesis in not overly complex, it contains some hazards and will take a good deal of laboratory skill, some sophisticated equipment, and a couple of days to complete. Please use caution when testing the final product - it is always best to start off with minute amounts and build dosage slowly so as to minimize any unforeseen adverse effects. 2CB is not exactly easy to make, but it is pretty straightforward. There aren't any very tricky reactions or especially messy procedures and the chemicals are not particularly suspicious to obtain (anymore than anybody buying chemicals or lab equipment today is suspicious to the authorities). But, like any synthesis of this nature, patience and precision are most imperative. Be sure to make the measurements exact, keep temperatures precise and check the colors or consistency of all intermediates. A general chemistry background is also very helpful, but not necessary if you lake the time to learn about what you are doing. ____________________________________________________________ The basic precursor for synthesizing 2C-B is 2,5-Dimetoxybenzaldehyde (2,5-DMB). Although you can even make this compound, the procedure is fairly time involved. For our purposes, it is best to start off purchasing this material. The first procedure is to change the 2,5-DMB into 2,5-dimethoxynitrostyrene. We do this by heating a mixture of 2,5-DMB and nitromethane in the presence of a catalyst, ammonium acetate. Set up an apparatus for refluxing. 'Refluxing' is basically boiling a solvent in such a way that the solvent continually evaporates, condenses, and is turned back to the boiling vessel. To do this we set up the apparatus as shown. -------------------------------------------------------------------------------- Click for small image (http://www.lycaeum.org/drugs/Phenethylamines/2C-B/synthesis/reflux-thumb.jpg) Click for larger image (http://www.lycaeum.org/drugs/Phenethylamines/2C-B/synthesis/reflux.jpg) -------------------------------------------------------------------------------- Place 100 grams of 2,5-DMB into a 500 ml flask and add 200 grams of nitromethane. Most of the solids should dissolve but if they don't immediately, don't worry - they will, once you start heating them. When most of them are dissolved, add 10 grams of ammonium acetate. Place the flask into an oil bath on an electric hotplate, connect the condenser and start a slow water flow through the condenser. DO NOT use open flame in any of these procedures. Nitromethane is very flammable! It is, in fact, rocket fuel. It's dangerous enough using an electric hot plate because of the sparks produced when the thermostat clicks on and off, but if you keep reasonable ventilation and a watchful eye on things, you should be okay. Turn the stove up to about 100 degrees celsius, the boiling point of nitromethane, and adjust it until the solution is boiling nicely. In a short time the color of the solution will turn yellow. Four hours later, when you are done refluxing, the color should be a deep red. Immediately set up for vacuum evaporation. If you let the solution cool off too much it may spontaneously crystalize, making it more difficult to purify, so do a little planning ahead of time. Turn the heat off, detach the condenser from the flask and add a few boiling chips to mixture. Boiling chips provide a very large surface area for lots of small boiling bubbles to form. This will keep the solution boiling smoothly without any "bumps" or big erratic bubbles. Connect the vacuum hose and apply a vacuum very gently at first and build up to a rolling boil without boiling up into the hose. As the solution evaporates, the flask will cool down and you will have to adjust the heat of the hot plate to keep a steady boil going. Eventually, you will remove enough solvent and the whole mass will crystalize into bright pumpkin-orange crystals. Turn off the heat and remove the vacuum hose from the flask. Always remove the hose from the flask before turning off the water. Otherwise, as the pressure drops water may be sucked into your product. Add 100ml of boiling isopropyl alcohol (IPA) to the mass and stir it as well as you can, breaking up all of the clumps. Your hot plate may still be hot and if you are working near it be sure NOT to splash any of this nitrostyrene onto the hot surface. The resulting fumes are a very potent teargas, something you don't want to experience! Let the flask cool and then pour off the red-colored alcohol solution. Add another 100ml of boiling IPA to the crystals and rinse as before. Rinse at least two more times or until needle-like crystals form out of the amorphous orange mush. Filter these crystals off and air dry completely. There must not be any alcohol left in the crystals, as this will ruin the lithium aluminium hydride (LAH) in the next step. This is 2,5- Dimethoxynitrostyrene (2,5-DMNS). Dissolve 50 grams of 2,5-DMNS in 300ml of anhydrous (dry) THF. If you cannot find anhydrous THF, then you will have to dry it the best you can. Do this by adding a drying agent (such as Drierite, or anhydrous Epson salts, or Silicagel) to the THF, let it sit overnight or longer, and then filter it out. This should get most of the moisture out of the THF that would otherwise ruin your expensive LAH. Arrange your refluxing setup with a 2-liter, 2-neck flask in the oil bath, a magnetic stir bar in the flask and a drying tube attached to the condenser. This can be a spare tube, plugged with cotton and filled with Drierite, that is attached to the open end of the condenser to prevent moisture from the air entering the reaction. Put 750ml of dry THF into the two neck flask and start to stir at a slow speed. SLOWLY add 25 grams of LAH to the stirring THF, NOT the other way round (LAH is nasty, dangerous stuff. It ignites in the presence of water, it's poisonous to breathe, to touch etc. Read up on it...). If you start adding the LAH too fast it may spark, so take your time. It fuzzes as it hits the THF, so add it carefully and let it easily mix into the THF. Now you are going to add your nitrostyrene solution. This is the reason for the two neck flask. As you add this to the swirling THF, it fizzes up pretty vigorously. Heat is generated and the THF starts to evaporate. Get the water running through the condenser and carefully add a little of the nitrostyrene solution (2,5-DMNS) through the extra neck. When the fizzing starts to catch up with you, stopper the neck up quickly to keep the fumes from escaping and let the reaction calm down and cool down a little. Repeat this many times until you have added all of the nitrostyrene. When you are done you should have a dirty gray solution fizzing away nicely. Slowly raise the temperature until reflux is reached and hold it there for 24 hours. Turn off the heat but leave the stirrer on and let the flask cool down. Once cold, SLOWLY add isopropyl alcohol (IPA) dropwise to neutralize any excess LAH. This will cause considerable fizzing. Make sure you are stirring while you add the IPA; if not, a layer of IPA will form and then any stirring that is done will result in the whole solution jumping right out of the flask. Take your time with this until there is no reaction with the addition of any more IPA. This gray aluminium slush is nearby impossible to filter out of the solution, but with the addition of 5Oml of 15% NaOH it becomes a white solid, and quite filterable. Now filter out the solids (you will be keeping the THF solution), and then wash the filter cake with a little extra THF. Combine the THF filtrate and the washings into a boiling flask. Now you must remove the THF from the mixture. This is done by simple distillation under vacuum. Set up the apparatus as shown. Add a few boiling chips to the flask and place it in the oil bath. Start the vacuum and increase until full strength is reached. As the THF evaporates, the flask cools down and needs more pressure to cause boiling. Finally, use the hot plate to cause steady boiling. Eventually you will be left with a dark-brown/goldenish oily residue. This is very crude 2,5-dimethoxyphenethylamine, also known as 2C-H, which you need to purify. Suspend the oily residue in 1 liter of distilled water and make it slightly acidic (pH of around 4) by adding HCl. The 2,5-DMPEA will become a water-soluble hydrochloride salt and dissolve into the water; other reaction byproducts will remain water-insoluable and can be easily removed. Add the solution to a suitably sized separation funnel and add 50ml of methylene chloride. Shake vigorously and let the phases separate. Drain out the methylene chloride. Repeat this washing with three more 50ml portions of methylene chloride. This should remove much of the solution's color and it will remain only slightly yellow. We must now freebase the solution before our final purification by fractional distillation. Make the solution very basic by slowly adding a strong solution of NaOH. The mixture will immediately take on a milky appearance. Shake the mixture vigorously for a few minutes to make sure the 2,5-DMPEA.HCl is converted to the freebase. This freebase is a dark oil which will separate and start to settle out. Extract the oil by washing, as above, with portions of methylene chloride, but this time keep the washings. Combine all the methylene chloride washings and remove the solvent by distillation as above for removing THF. You will be left with around 50ml of a dark oil. Now we will distill the oil under reduced pressure and at a relatively high temperature. To do this we use a slightly different setup than the one used to remove the solvents. We won't need the condenser in this case and the flask should be much smaller (around 100 to 250ml) to adequately accommodate the smaller volume of oil. Setup the apparatus as shown. Make sure you use a water trap. Any cold water entering the system will crack the flasks and ruin the procedure. Also make sure to add boiling chips to the flask. Oils tend to really spatter and the chips are absolutely necessary. Bring the system up to full vacuum slowly. There will probably still be some methylene chloride that will boil off and end up on the receiving vessel. This is ok. As we heat the system it will eventually evaporate out of the flask. At full water pressure on the aspirator, the oil bath will need to reach 195 Celcius before the 2,5-DMPEA will start to come over as clear, waterlike oil. Keep the temperature and pressure constant as the oil slowly drips over. This will take some time depending on your exact setup. When you are satisfied that you have distilled out all the product turn off the heat and disconnect the vacuum from the flask. You should have around 20 grams of pure water-white 2,5-DMPEA. (2C-H). -------------------------------------------------------------------------------- Click for small image (http://www.lycaeum.org/drugs/Phenethylamines/2C-B/synthesis/distill-thumb.jpg) Click for larger image (http://www.lycaeum.org/drugs/Phenethylamines/2C-B/synthesis/distill.jpg) -------------------------------------------------------------------------------- Now we will brominate the 4 position of the benzene ring of our 2,5-DMPEA. We do so with pure elemental bromine.,a fluid. Bromine is by far the nastiest stuff you'll ever want to come across. As soon as you open the bottle it will start to crawl out. If you noticed how well packed your bottle of bromine was, you were probably expecting something like this. Use this only in a fume hood if possible. Don't even open the bottle in your house or the whole house will smell like bromine for days and days. Fortunately, we don't have to deal with it for very long. If you have no access to a fume hood (which is probably the case) then at least pick a well ventilated area, away from any nosey public, and have a large jar with an airtight seal available. Place your 2,5-DMPEA in a 250ml beaker and weight it on a digital scale. Add to it, this same amount of glacial acetic acid. Place another 250ml beaker on the scale, quickly open the bromine and weigh out the same weight as your 2,5-DMPEA. Add to it that same amount of glacial acetic acid and quickly add the 2,5-DMPEA solution to it. After a few quick stirs, seal it in the large airtight jar. The beaker will heat up but it shouldn't be a problem with these quantities. If you scale this up you may need to rig up an external cooling water bath. Light yellow solids will slowly form and in a few hours the solution will cool down. The beaker should pretty much now be solid with light yellow crystals of 2CB-HBr. This 2CB-HBr has many associated forms involved with it and for a consistent, predictable drug we will need to convert it into the hydrochloride salt. Take the whole mass of 2CB-HBr and filter it. Rinse a few times with cold glacial acetic acid. Place the still-wet crystals into a 500ml beaker and slowly add a 40% NaOH solution. Stir briskly and a dark oil will start to settle out. Separate this oil, as you did above, by extracting with methylene chloride. You will also distill this oil, under pressure and at high temperature, as you did above, and again collect a clear oil. This is pure 2CB freebase. The final step is making the hydrochloride salt of 2CB. This is done very easily. Since 2CB is not soluble in water, we don't have to worry about completely anhydrous solvents that are usually the case when crystallizing the final products. Add the freebase oil to lOO ml of distilled water and slowly add acetic acid while stirring until the freebase dissolves. This won't take very much acetic acid. Get this solution stirring with the magnetic stirrer and slowly add concentrated HCl. A white precipitate of 2CB-HCl will immediately form. Continue to add the HCl until the solution is thick with fine white crystals. Stop the stirring, and when the crystals settle out, decant the water into another beaker. Add a little water to the crystals, stir and let settle. Add this wash to the beaker with the original decanted solution, put it back on the stirrer and add more HCl. More crystals should form. Repeat this process until you are satisfied that all the crystals have formed. Now add all the crystals together - add water, stir, let settle and decant repeatedly until the wash water has a fairly neutral pH. Now you can filter the crystals and air dry. This is fairly pure 2CB-HCl. Enjoy. Dosage: in PIHKAL, Shulgin recommends 12-24mg, which is a good range to work with when taken orally. An alternate means of administration is by sniffing. I have found this much more effective. Cut the dosage in half and expect to feel results within 10 minutes or less! Note: Sniffing can be very painful! It's best to do smaller amounts than the whole dose all at once. As know from above, 2CB is not water soluable and will sit in your nose burning for a while - and it does burn. But the pain goes away in short time and the results are worth it. Experiment! -------------------------------------------------------------------------------- Reaction Mechanisms : -------------------------------------------------------------------------------- Click for small image (http://www.lycaeum.org/drugs/Phenethylamines/2C-B/synthesis/chem-thumb.jpg) Click for larger image (http://www.lycaeum.org/drugs/Phenethylamines/2C-B/synthesis/chem.jpg) --------------------------------------------------------------------------------  HTML by: Andrew Edmond (Removed many typo's and added some minor notes to this well written synthesis, LT/) Made possible by: Lycaeum Drug Archives -------------------------------------------------------------------------------- ADDENDUM : See the "New IDEAS from ALL !" thread in the Newbee forum for some additional info. And I should be more then pleased to get more info from all of you, where to find the good 'recepeaces' LT/ Everybody, I would be glad if you hop in this thread ( but then the one situated in the Methods forum, so this one will stay clean, after each update !)from time to time to assist with rewriting or finding any blatently errors, I'm only human, you too want good write-ups so nobody get hurt in exploring their hobby. I'm glad this edit-addy works, I'm intending to do a lot of work in this thread the coming time, I intend to make it a sort of fast introductory booklet for all those people hanging around without the faintest knowledge of chemistry, so we will be spared from all these beginners questions for posted methods, and we have some more time for ourselfs then, just refer to this thread when questions come up which are solidly answered in here. I want to gather ALL working methods in here (mentioning the originators of course, to give credit to whom it belongs) , edit them a bit for readability, and after that going to add a extensive Lab Manual as an Addendum.   Rhodium (Chief Bee) 07-06-00 03:05 This will be added to my page. http://rhodium.lycaeum.org/ WISDOMwillWIN
	Synthman (Hive Bee) 07-01-00 05:09 No 23589		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			Thanks LaBTop, I've been interested in the performic oxidation for a while now. Good writeup, Synthman Post merely for informational purposes. I haven't done anything illegal and nor should you.
	bizwax (Hive Bee) 07-01-00 08:55 No 23624		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			Excellent writeup LaBTop. I've learned some new lab tricks just by skimming already. I presume that this method is used when your ready to scale up? Is that the advantage to using it?  (I can just picture little ol me (85lbs - 4'8") in the lab trying to wrestle with a 22L flask and my mother coming out to the lab and catching me during that moment :) )
	blaztoff (Hive Bee) 07-01-00 13:44 No 23707		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			Thanx labtop. That just solved a problem i was having. Great info on the whole process and insight on scaling up. I was a little worried all the info i had talked about a reaction that was ussless when doing over 25grams. TTTHHHHAANNNKKK YOUUUU
	Headgames (Stranger) 07-01-00 21:13 No 23812		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			Thanks man!!!! Very Informative.
	Stonium (Moderator) 07-01-00 21:55 No 23825		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			Oh Daddy. It's just wonderful!
	LaBTop (Stranger) 07-05-00 12:02 No 25164		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			METHAMPHETAMINE PRECURSORS CLEANING/WORKUP Extractomania........by Ozbee and friends..........edited by Placebo INDEX: 1: Equipment 2: Ingredients 3: Method step 1: step 2: step 3: step 4: step 5: step 6: 4: Acid/Base 5: HCl-Gassing 6: Notes 1: Equipment * Various jars, glass vessels, beakers etc * PH paper, or electronic PH tester * Filter paper or coffeee filters * A strainer that will fit your filters nicely, so that you get better surface area then a funnel * Hair dryer, or heat lamps * Hot plate, no open flames, only heat elements * Seperatory funnel, or similar, or tube to siphon 2: Ingredients -Pills containing psuedo-ephedrine HCl or ephedrine HCl. -NaOH/Sodium Hydroxide/caustic soda/strong base/lye. -Epsom salts that have been baked in oven (200c) for an hour to dry. -Methanol -Acetone -Toluene -Distillated water 3: Method ***note*** : If pills have red coating, put in jar, with acetone, shake until red coating is dissolved and then continue as below. Step 1: First, put your pills in a jar. Add methanol about double the volume of the pills. Cap the jar and shake till they break apart. Leave to sit for a few hours shaking every 1/2 hour. Let settle into 2 nice layers then siphon or decant off top layer. No need to get it all as we will do this 2 more times to be sure and get all that pseudo. step 2: Once you have done it 3 times and have the 3 lots of methanol from above, put them together and put in freezer. You want to get it real cold, near freezing and then filter it thru a very fine filter, this may take some time if you don't have a vacuum filtration setup but thats ok, we aint in a hurry. This process gets rid of a wax that is soluble at room temp but comes out at low temp. step 3:***note*** : This step is not necessary and only speeds things up. After the chilled filter, we will reduce the volume of methanol/pseudo solution. So, with good ventilation and a fan blowing over pot, just reduce the volume of methanol, but not till you see crystals or anything. Just reduce it to a manageable amount, we just want a saturated solution, you'll notice it thicken a bit. Stop, take it off. step 4: Now you want to pour a thin film of this methanol/psuedo solution out on a mirror or glass table for fast evaporation, or you could just leave it laying around a couple of days and let nature take its course, and it does make pretty crystals. Scrape all your crystals up when they are dry and put into another clean pyrex vessel. step 5: Now pour Toluene, about double your psuedo volume (**dry/anhydrous<<use your epsoms!**) over your powdered psuedo, and heat till just before boiling with your fan blowing over it. Boil for 5 mins and then filter. Repeat this with fresh toluene until when you boil toluene it stays clear. To be sure of toluene doing its job, after filtering, add water to toluene before discarding and you'll see the shit come out. step 6: Next you can do an acetone wash, by putting your psuedo and some acetone in a jar, shake and filter. Dry pseudo and you should have fuckin clean pseudo HCl...... This procedure, rids the pills of: MCC waxes polymers lactose and most shit! BUT, not povidone! More on that later. You may choose to react your psuedo now. Or do an A/B (acid/base) extraction, basicly turn it into a freebase, or oil. Keep in mind..If you do an A/B now, you may lose some psuedo to the povidone. So what are the choices? Well, povidone is known to go thru Hi/RP, no problem, but must be steam distilled out after. Which is a good thing coz you got no seperations or emulsions and the cleanest meth around. Povidone is bad because povidone is known to absorb and hold amines. It depends on what reaction your doing! 4: A/B: Ok, get your nice dry white powder and add about equal part water. Now make up a 20% NaOH solution (or 4 parts DH2O:1 part NaOH). Add Toluene to water/pseudo solution about equal to water volume. Yes, toluene first, it gives the pseudo somewhere to go instead of being burned by the base which can break it up and turn it into aziradines!(toxic)! Add NaOH solution to water/pseudo/toluene solution till PH 13, and remember to test PH of water not toluene! Now shake the jar up very well and let settle into layers. Seperate toluene layer. Repeat this process 3 times and combine all your toluene. You can wash the toluene/pseudo freebase with water now, if you like, and seperate again. Now you can either, evaporate toluene for freebase crystals, or you need to turn the freebase into a Hcl salt again. So you can add fresh DH2O (about 2mL for each gram of pseudo) to your toluene and drop HCl acid slowly with shaking each time into the toluene. Check pH all the time and stop just before neutral. Shake again, and recheck, this is very tricky and takes patience. Now seperate the water from the toluene. Now you can evaporate your water to get your pure pseudo HCl. You can repeat this another 1 or 2 times and get a little more. 5: Gassing, Gassing makes things easier coz you just gas it, filter and there'r your crystals, but it is tricky to get the hang of it and Hydrogen Chloride is dangerous! It will burn your fuckin lungs instantly if inhaled too much of it! You need to pipe HCl gas into your jar full of toluene and pseudo freebase, but the gas and your toluene must be dry : no water, or everytime the gas forms crystals it will be reabsorbed by the miniscule amounts of water. If you don't know how to extract, you shouldn't play with gas yet. If you know how to gas then read on... So, you need to dry your toluene/pfed solution with pre-baked epsom salts to absorb the water, and then filter them out. Then gas your solution and you will see a snow storm before your very eyes. Then just filter and dry crystals. But still may contain povidone. Post merely for informational purposes. I haven't done anything illegal and nor should you. ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ METHAMPHETAMINE SYNTHESIS I.----Placebo's compilation of "the Cure" by Ozbee (clean-up of sudafed and other ephedrine pills) and various RP/I2(red phosphorous / elemental iodine, pure, crystals) methods. placebo (Hive Researcher) 07-04-00 11:04          Go to Whoah!    Ok, this is a compilation of many peoples' methods. I believe this to be the best, simplest, fastest, and cleanest method for producing meth-amphetamine, in the highest yields possible for RP/I2/E reaction. Remember, each and every step gives small losses, and this method has the least steps! It is a culmination of efforts by Worlock, CHEMMAN, and maybe a few tiny touches by me. I re-iterate, I don't want any congratulations except for the write-up itself. You will need these things, and no substitutions allowed. If you can't get this shit, you ain't ready to make the best Go-Go in town. This is a refinement of all methods, and the next step up from Push Pull, but nobody should be discouraged from attempting this, as you will probably find it easier. pH paper isn't even necessary. This post is one method from Go to Whoah. This post has to be followed from Go to Whoah. Otherwise you can run into trouble, as povidone is not removed in this extraction. It will be removed at the end. Each step was chosen to complement the next. Understand? Read on..... Index: 1: Equipment 2: Reagents 3: Extraction of pfed 4: Reaction 5: Steam distillation 6: Crystallisation Equipment: Various jars 2L pyrex vessel 2L 2 neck round flat bottom flask 1 condenser, I recommend a coil condenser but a Liebig will suffice. 1 sloping splashhead or better, a steam distillation sloping splashhead. A steam pressure cooker, that has a release-valve on top. Hotplate, electric of course. Filter paper, Buchner and vacuum would be nice too. Thermometer. 1 Glass stopper. Lengths of clear pvc tubing. Pot with vegetable oil, which can fit your reaction vessel. Reagents: Iodine crystals. Red Phosphorous. Pseudo-ephedrine, or ephedrine. Methanol. Toluene. Acetone. NaOH. All must be clean and anhydrous. Ice. Extraction of pfed: This method will deal with the HCl salt of pfed, and a streamlined version of "the Cure". All pills are dumped into a large jar and double of this pills-volume in the form of methanol poured on top. This is stirred vigourously and let stand to settle thereafter, in the fridge seems to speed it up. After the top methanol layer has cleared it is carefully decanted off. This procedure is repeated 3 times. All methanol pulls are put together and the methanol boiled off on a hotplate. As methanol gets down to the last little bit, it is taken off the heat. Then a portion of acetone, twice your remaining liquid is dropped in. This forces the pfed crystals to crash out. Then the remaining liquid is carefully evaped off. Washes: Now you have your crude/dirty pfed HCl. Next we will be doing successive toluene washes. Put your pfed crystals in a pyrex (heat proof glass). Now add toluene to a safe level that can be lightly boiled on the hotplate. After about 5 mins boiling with stirring, take off the heat and let it settle a minute. Now carefully pour off toluene into a filter to catch any remnants of pfed that may follow. Now if you get the toluene that has our contaminants in it and add some water, you will see the crap, crash from the toluene into the water.This is the crap that came thru with the methanol pull. So as we continue to do multiple toluene washes, we will continue to test the toluene after pouring it off, to see how we are progressing with the cleanup. When we have reached a point where no crap comes out of the toluene, with the addition of water, then we are ready to try acetone. Usually about 3 boils in toluene, but of course it depends how much you'r using. So, as before we will add a portion of acetone and boil lightly. Now when we pour off the acetone, we will add a tiny amount of water and some NaOH. This is our final test, when you do this and no crap falls out of acetone you are ready. This will be the cleanest pfed you have ever seen, guarenteed! AND, yields should be >90% if you'r carefull! 95% is good. Reaction : Smallest reaction to be attempted, especially by newbees, is 1 oz of pfed, so that even taking into account sloppiness, lack of experience and losses along the way, you should get some product. Ratios of reagents are: 3:3:1 or 1:1:1/3 , ie.E:I:RP aka, equal amounts of Iodine and pfed, and a one third amount of RP. This is calculated on a weight basis, and can be scaled up or down as necessary, e.g.60gmE/60gmI2/20gmRP or 120gmE/120gmI2/40gmRP etc etc. First prepare yourself an icebath. Yes, icecubes and water in a sink or bucket. Now, many will say you should add this first or that first. Well, after much reading of different peoples methods, I say.... Chuck the whole shebang in together, while your flask is on ice, lift and swirl ingredients together, while maintaing on ice. Put your condenser on top and start water running thru, from bottom to top. Now, the idea is to get the reaction going in the most controlled way possible, you want to let the reagents react in the container vessel fixed in the icebath, if at all. Then move vessel from icebath to room temp. If things look like they're going too fast, put back in ice bath, you want to keep the reaction going but only at a nice slow, controlled pace. This is also necessary to control vapour in the condenser! Thick and or dis-colored smoke is bad, and plumes of smoke will escape from condenser. Let things progress at a nice slow pace, as things slow too much, you can start applying heat. So prepare an oilbath and bring to about 50 C, if there is no more action in your vessel. You can move it to the oilbath, and the same goes for it as before, when things slow down. Adjust heat up, to say 100 C then 150 C for one hour, to make sure reaction has completed. The whole time you should be watching to keep a nice reflux going, and not too much vapour is escaping from condenser. Now remove from heat and disconnect condenser, add ice water to quench reaction. The reason for ice water is to calm the reaction down when NaOH is added. Its up to you if you want to filter out RP or leave it in untill the end. I would leave it, it will be washed nicely by next process and be easier to filter. Now add lots of NaOH to bring reaction mix to + 14 pH. You cannot over-basify, as meth won't be destroyed, its a tough MF! Steam Distillation : Now you need to set up your glassware for steam distillation. Attach the steam distillation sloping splashhead to top hole of flask, attach plastic hose to steam inlet and the other end on the release valve of the pressure cooker that is full of water. Attach condenser on the end of splashhead, and rig the whole up so it stays up. Place a jar at the end of condenser to catch our distillate. You want to heat both the pressure cooker, and the reaction flask. Sit back and get ready for one of the most beautiful sights and smells. The meth freebase that is sitting on the top of your aquaeous layer in the flask will vapourise and be carried across and be condensed in the condenser and trickle down into your jar. It will sit atop of a bottom layer of water. After the last of the oil has come across, change jars and leave the setup to run for another hour, just to make sure you got it all. Any povidone from the pills will be stick behind in the reaction vessel. It has been noted that some polymer that may have been left from extraction, may follow the steam. Crystallisation : Now we have a jar of water, with this sweet clear oil sitting on top. Next options are to add HCl acid slowly with stirring until the oil layer disappears, and then evap the whole lot to get crystals. Or, as I found, you may have some polymer that has come over with the steam, and is now sitting in the water layer, and it looks cloudy. I don't want to evap all that, it will just concentrate the shit in there, (plus its very time consuming evapping water, plus you risk losing some meth as the water evaps). I think you should just throw a little toluene into the jar, and then seperate. Now your absolutly pure meth freebase is in your toluene! Now you can either gas, for instant the now clean meth, or add minimal distillated H2O and then acidify to pH 7, shake, seperate and evap water for crystals. Repeat this step if you do it this way, as some more may come in a second go. With this process from start to finish, you shouldn't need to re-crystalize, as your product should be the cleanest shit anybody has ever seen anyway. But you may want to, for the purpose of growing nice big crystals. In which case, add just enough hot methanol to dissolve all your meth and then place in freezer. The secret is, the slower the evap, the bigger the crystals. So a nice slow room temp evap over several days might be fun. Enjoy, and do not attempt anything above, before you completely understand what you are doing! You must have a sound understanding of the basics first! ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ ------------------------------------------------------------------- How to produce anhydrous (= dry = waterfree!) HCl gas using no special equipment for all your amination steps of freebases - by Psychokitty. ------------------------------------------------------------------- To date I have never used Strike's and Fester's method for producing HCl gas. Reasons for this are as follows: 1. The necessity of laboratory glassware (no OTC hardware). 2. What seems to be a messy proceedure using table salt (but I wouldn't know exactly as I've never tried it). 3. Difficult dismantling process (at least it seems to be more difficult than mine). I don't remember the exact journal reference that inspired my method, but I do know that it is described somewhere in Inorganic Syntheses Vol. I. Okay. First, here is what you need: 1. Beer bottle (transparant). 2. Plastic baby syringe (15 ml capacity) found at the pharmacy section at any grocery store. 3. Four or so feet of ice-maker transparant-white polyethylene tubing found at the hardware store. (I don't remember the exact diameter size. All I know is that it IS the smallest size available.) 4. One table-leg stopper (rubber, beige or black). Another item of which I don't know the size. Just take your beer bottle into the hardware store and see which size fits snuggly on its top. 5. One aluminum tube that is the exact diameter size as the polyethylene tubing. Found at the hardware store but don't know what they are used for. They are sometimes made of brass. 6. One bottle of sulfuric acid drain cleaner. 7. One bottle of concentrated hardware store muriatic acid (32%?) Assembling the HCl generator is easy. 1. Use the aluminum tubing to burrow two holes to the top of the table-leg stopper. Use a twisting motion while appling pressure for about a minute and eventually the tube will pop through. 2. Place the table-top stopper over the top of the beer bottle. It'll fit snugly. 3. Insert the polyethylene tubing into the middle-most hole and push through until the tubing hits the bottom of the beer bottle. With scissors or a knife cut off the polyethylene tubing about two inches from the top of the beer bottle. 4. Take the entire table-top stopper inserted with the polyethylene tubing off of the beer bottle. Pour into the beer bottle a volume of sulfuric acid about an inch high off of the bottom of the beer bottle. 5. Replace the table-top stopper/polyethylene tubing on top of the beer bottle. Insert the remaining tubing into the last hole of the stopper until about two inches into the bottle. Cut tubing down to desired length. 6. Pour about twenty milliliters of concentrated HCl into a cup. Extract into baby syringe until syringe is full (15 mL). NO, the HCl will not dissolve any part of the syringe in any way. NEITHER THE HCl NOR THE SULFURIC ACID WILL REACT WITH ANY PIECE OF HARDWARE USED IN THIS SYSTEM. THIS SET-UP HAS BEEN TESTED MANY TIMES WITH SUCCESS. 7. Insert the syringe into the middle tubing (the one that extends to the bottom of the beer bottle. End should be submerged in Sulfuric acid.) If insertion is difficult, use a knife to scrape the inside of the tubing to allow the syringe to fit more easily. 8. Securing the set-up with a clamp of some sort attached to a stand is optional but desirable. 9. Have handy on the side a container full of water. The use of this set-up to gas ones solvent/amine is just as easy. 1. With right hand, hold the tubing that will expel gas and lower into the solvent/amine solution. 2. With left hand slowly start to inject the HCl solution in the syringe into the sulfuric acid. Once it hits the acid, there will be alot of fizzing and foaming and IMMEDIATELY HCl gas will be pumped into the solvent/amine solution. Foaming is sometimes a problem as it starts to reach the top of the beer bottle. Simple wait a while and let it settle and then continue. Sometimes certain brands of drain opener can cause excessive foaming. If this occurs, switch brands. 3. One syringe is usually enough for an amount of about 30-40 g of product, but if more is needed after all the HCl has been injected, slowly SLOWLY remove the syringe from the tubing, first be letting a crack of air into the system. BEWARE that this is suddenly going to bring a minor rush of HCl from the gassing tube so make sure that it is submerged when doing this step. To continue, refill the syringe and proceed as described above. 4. Once the gassing is complete, leave the syringe ATTACHED to the injection tube and submerge the gassing tube in the container full of water (If the syringe is not attached to the injecting tube, the following sequence will not occur). Weigh down the gassing tube somehow as it must remain submerged. In a few minutes (about five) the sulfuric acid will cool a bit causing a sucking-back of the water into the beer-bottle. This will happen very suddenly and very fast, but not to worry as the water will only go in as far as the top of the beer bottle. This is actually an advantage as in this way one is able to dilute the remaining HCl gas AND the remaining sulfuric acid. Of course the bottle will get hot but if left aside for a few minutes it will eventually cool making opening the container and dispensing with the acid solution an easy task. If the bottle is opened for whatever reason without the above acid dilution step, HCl gas will be everywhere. Hope this method will prove useful to you my fellow bees, it sure has been for me! ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~
	Rhodium (Chief Bee) 07-06-00 03:05 No 25428		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			This will be added to my page. http://rhodium.lycaeum.org/
	chemistrystudent (Newbee) 07-07-00 09:12 No 25900		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			It's good to see that interested parties can now follow a larger scale synthesis. Thanks you your input LabTop! Now maybe I'll make a video of this synthesis for the NewBees. Just Kidding!! Well, I thought it was funny. "Life is a boomerrang what you throw out will always come back"
	ikb3 (Stranger) 07-09-00 00:29 No 26595		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			Would you please explain how 100% pure Sassafras oil is refined to obtain Safarol? If you can not, would you please refer me to where I could read up on the methods> Thanks ikb3
	LaBTop (Moderator) 07-09-00 12:12 No 26726		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			Even when you think you made it as clear as you can, still questions arise which I would not have thought of, because I see it as common knowledge. In that sense your question is helpfull, it let me realize that non-chemists do not know that there is no 100% Sassafras oil, it's allways a mixture of the essential oils at present in the extracted plant material, and differs from geografic situation to situation. Brazil and Vietnam seem to have the best and relatively high safrole contents, 75 to 90 %, which means they are lucky to have the good trees there and use good extraction techniques, like steamdistillation and vacuum destillation thereafter. I will change above text to : Sassafras-oil, usually etc. xx % safrole oil. ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ Methyl_Man (Hive Researcher) 06-05-00 10:40 : METHYL_MAN's WRITEUPS of MeOH BENZO WACKER and MeNO2-Al-Hg. Consult these threads to avoid unnecessairy questions : http://rhodium.lycaeum.org/clandestine/gonzo/index.html Post No 13991 and Post No 15667 and Post No 31473 --------------------------------------------------------------------------------------------------- Here they are, with minor changes from older versions for greater accuracy. =========================================================================== Methyl Man's MeOH version of the benzoquinone wacker : Materials: 400mL MeOH (methanol) 50mL distilled H2O 150g p-Benzoquinone 2g palladium (II) chloride (PdCl2) 178g safrole DCM (methylene chloride; dichloromethane) NaCl (non-iodized table salt) Sodium bicarbonate (baking soda) 5% NaOH HCl (hydrochloric acid, from muriatic acid) Magnesium sulfate drying agent (epsom salts baked in 400¢XF oven for 2 hours) Method: 1. In a 2L flask fitted with a reflux condenser and addition funnel place 400ml MeOH, 50ml dH2O, 150g p-Benzoquinone and 2g PdCl2 and leave to stir for a minimum of 60 minutes. Note that a recent improvement has been discussed which involves stirring the PdCl2 in the solvent (MeOH in this case) for several hours before adding the water and benzoquinone. It is likely that this does enhance yields a bit by ensuring maximum efficiency of the PdCl2's catalytic action. Either way will work well, however. If you let the PdCl2 stir alone for a while, when you then add the water and benzoquinone, let them stir for an hour as well before beginning the next step so as to ensure complete dissolution of the benzoquinone. 2. Place 178g safrole mixed with a bit of MeOH in an addition funnel. 3. Add safrole dropwise from the addition funnel over 60 minutes or more. However, when the addition is about 80% finished, apply low heat just sufficient to start a mild reflux (cold water through the condenser). 4. After the safrole addition is complete, leave mixture stirring and  refluxing for 8 hours. (If you must stop at this point and resume another day, be sure to put the mixture in the freezer, sealed well. The raw ketone decomposes unless stored at freezer temperatures.) 5. Filter out the solids present in the mixture, which are hydroquinone (the degradation product of the benzoquinone) and PdCl2. This can be done by vacuum filtration or by simple gravity filtration with coffee filters. Many prefer gravity filtration with this synthesis because the solids produced in this reaction are very fine and are problematic to filter with vacuum. Don¡¦t try to recycle the PdCl2, as it is too difficult to separate from the hydroquinone to be worthwhile. 6. Flood mixture with 1.7L 3N (~10%) HCl. (Here's the quick math: add 500mL of 31% HCl [muriatic acid] to 1150mL H2O to get 1.65L ~10% HCl, close enough for this purpose.) 7. Extract flooded mixture with 3 portions of DCM (1 x 500mL, 1 x 250mL, 1 x 100mL) in a large separatory funnel. The desired raw product, MDP-2-P ('ketone'), migrates into the DCM as an oil. Separate the DCM/ketone layers and combine them. (Note: when you first hit it with the DCM you will probably observe a bit of scum which will float on top of the water layer, which will work its way down during these three extractions to appear as a blob of spongy semi-solid interface. It¡¦s actually very mobile and easy to work around; simply avoid allowing it into your DCM separations. The same thing will happen in your washes in steps 10, 11 and 12 below, but by then you will be quite the pro at working with it.) 8. Extract water layer with a final small amount of DCM. 9. Add this final small DCM extraction to the combined oil/DCM solution from step 8. 10. Wash the ketone/DCM solution with saturated sodium bicarbonate in water twice (500mL each wash). 11. Wash the ketone/DCM solution with saturated NaCl 3 times (400-500mL each wash). (Note: as you do these bicarb and salt water washes, you should be seeing the ketone/DCM solution getting progressively more greenish colored; this is visible in the film of solution that runs down the inner surface of the sep funnel). 12. Wash the ketone/DCM solution 3 times with 500mL 5% NaOH (500mL each wash). If you did step 5, you will have a very easy separation. (Note: you should also see a very noticeable color change upon doing the first of these three washes wherein the ketone/DCM layer becomes a strange, thick reddish-brown, almost orange color. This happens as the NaOH pulls the majority of the solvated hydroquinone into its layer, cleaning the ketone. The NaOH layer in the first wash will be very dark brown, almost black in fact. The next two will be a far lighter, watery, orangy color.) 13. Dry the ketone/DCM solution with ~50g magnesium sulfate. 14. Distill off the DCM using mild heat on a water bath and ice-cold water through the condenser. This will take several hours. 15. Add 50mL of high-oleic safflower oil (no additives!!) to the ketone oil as a buffer to prevent the ketone from scorching in the distilling flask. 16. Vacuum distill the ketone/buffer oil mixture. This also will take a few hours, but not as long as distilling the DCM off did. 17. At 100 to 140¢XC (wherever your particular vacuum dictates), a minor amount of safrole might come over. If your safrole-to-ketone conversion was good, there should only be a very small amount. If it is only a few drops to a milliliter or two, you can leave it in, and not change/clean receiving flasks. If you are a stickler for purity, discard it. It will not harm anything later if you leave it in. But if it¡¦s more than a couple of milliliters, get rid of it. 18. At anywhere from 25 to 40¢XC above the temperature your safrole usually comes over with the same vacuum, the ketone should begin coming over. You should get about 100 to 120g ketone. The color of the ketone coming over will likely be a pale, fluorescent-looking greenish yellow. In fact it looks not unlike anti-freeze, similar neon green. You can stop distilling when the rate of ketone coming over has slowed to an agonizing one drop per 90 seconds or so. At this point there is so little left that it is probably not worth your time to wait for a drop per 1.5 minutes (it is not worth mine anyway). 19. Immediately store your precious fluid in the freezer in an airtight sealed flask or bottle. Happy cooking! --------------------------------------------------------------------------- The MeNO2(nitromethane)-Al-Hg reductive amination according to Methyl Man Since the appearance of Ritter's writeup of this method in Total Synthesis II, much discussion has taken place about it but, it has sometimes seemed, little has been clarified. This is due in large measure to the sensitivity of this reaction to even the most minor changes in its many variables. With this writeup, I hope to provide a clearer view of the method and to allow others to benefit from the hard-won experience of someone (not me)whom we'll call Mr. A. Ritter's original writeup, while inspiring, lacked details about the many nuances that, once understood, allow the amateur chemist to really understand this reaction's dynamics. Thus I have tried with this writeup to help the neophyte who has only physical observations and scant written material to guide him (although I suspect and hope that it may even help a few more seasoned cooks as well). The first thing I'd like you to look at is the array of interrelating variables in this reaction that make it so delicate. They are as follows: 1) the thickness/type of the aluminum 2) the consistency (i.e. flat, ground, etc.) 3) the amount of HgCl2 used in relation to the amount of aluminum 4) the addition rate of the MeNO2/MDP-2-P 5) the size of the reaction vessel in relation to the scale of the reaction 6) the ability to effectively stir the reaction 7) the coldness of the water through the reflux condenser (yes, even that!) The above factors are sort of submitted in an order of importance (#1 being most important), but in reality they are all inextricably related. I observed firsthand the trials and tribulations of Mr. A as he struggled to match up the correct combination of ratios and conditions that would allow a smooth, consistent reaction and predictable results every time. Finally, after lots of frustration, confusion, losses, and---in the end---a revelation, the perfect set of elements was hit upon and recorded. The scale Mr. A chooses to perform this reaction on is half-scale to the scale in the Ritter writeup, which was 55g aluminum and 50g MDP-2-P. Therefore this writeup will illustrate the reaction on a scale of 27.5g aluminum and 25g MDP-2-P. The subject found for his own personal reasons that this smaller scale was much easier to manage (not the least of which is that even with a huge 4-liter separatory funnel, at this smaller scale it gets pretty filled up!). There's no doubt that the original larger scale can be successfully applied, although it would require adjustments in the glassware capacity, stirring method, and probably other elements. MATERIALS and APPARATUS: --  27.5g Reynolds Wrap Heavy Duty aluminum foil --  25g MDP-2-P --  20 mL MeNO2 of 99+% purity --  750 mL MeOH + 50 mL more for addition funnel + additional small amounts that will be needed later to thin the mixture --  400mg HgCl2 --  2-liter 2-neck flat bottom flask --  reflux condenser (400mm preferable) --  250mL or 500mL addition or separatory funnel --  cooling setup (bucket, water pump, tubing, 1 large bag ice) METHOD: 1. Weigh 27.5g of Reynolds Wrap Heavy Duty aluminum foil (NOTE: it HAS to be Reynolds and it MUST be the heavy duty stuff) and then tear it by hand or cut it with scissors into small rectangles approximately 1" by .75". Settle down with this task with a good CD or TV show because it is tedious and may take about 1.5 to 2 hours. 2. With a coffee grinder, "grind" these pieces of foil for durations of about 10 seconds. Fill the coffee grinder only loosely (about two thirds full---don't stuff it! That will adversely change the consistency of the ground foil). It will probably take about 4 to 5 "loads" in your grinder to do the whole amount of foil, depending on the size of your grinder. (In actuality, the foil does not get "ground," but rather, each individual piece just gets compacted and compressed. If it is compressed too heavily, the inner surfaces of the foil nuggets may be rendered inaccessible to the Hg/MeOH solution, changing the timing of the amalgamation and maybe even causing an incomplete or failed reaction.) When properly done, the foil should be in gnarled little nuggets about the size of long-grain rice grains and should look really tight and small. The smaller, the better for good stirring. 3. Place a 3" stirbar in your 2L flat bottom flask and onto your stirplate. Add the foil nuggets to the flask and then proceed to set up your glass, support and clamps so that the reflux condenser and addition/sep funnel are securely affixed and your flask is well-centered on the stirplate (this will be critical when you begin to attempt stirring!). Also, prepare your cooling, i.e. attach the inflow and outflow tubes to the reflux condenser. 4. Carefully add the 400mg HgCl2 to 750mL MeOH to a tightly sealable bottle and shake to dissolve all HgCl2. Set this solution aside. 5. Combine the 25g MDP-2-P, 20mL MeNO2, and 50mL MeOH and pour them into the addition/sep funnel. Rinse your beaker (or whatever you used) with a tiny bit of additional MeOH to get the residual ketone and add it to this MDP-2-P/MeNO2/MeOH solution. 6. Very slowly and carefully (w/gloves, glasses, long sleeves and a Hail Mary if you're Catholic), using a large funnel, pour the HgCl2/MeOH solution from step 4 down the condenser. 7. Turn the stirring on full blast for a 5-second burst to intimately mix the solution and the foil. If you have prepared the foil as described above, it will easily stir. Give it a few more 5-second stirs over the next few minutes. I believe that doing this really helps facilitate the amalgamation process that is about to occur. 8. After about 5 minutes or so, you will begin to see bubbles popping up on the surface of the MeOH solution. At first they will be tiny, like champagne bubbles. Then after a few minutes you will see them joined by larger bubbles closer to the size of those seen in boiling water. It is around this same time that the appearance of the aluminum will change from its normal shiny silver color and start to take on a dull gray look, accompanied by a gray cloudy look that begins forming in the MeOH. This is the magic moment when you want to begin dripping in your MDP-2-P/MeNO2/MeOH mixture. Set a drip rate of approximately 2 drops per second at this point and no faster. You can speed it up a bit later to accelerate the reaction if desired. 9. Place about 3 lbs ice into your bucket. When you can feel exothermic warmth begin by feeling the outside of the flask, quickly add about 2.5 liters water to the bucket (or an appropriate amount to make very ice-heavy ice water) and plug in the pump. 10. While monitoring the growing intensity of the bubbling amalgamation, turn on/off the stirring intermittently as you did earlier. This time it is to assure distribution of the added ketone/nitromethane in the reaction flask but also because the amalgamation seems to gain its vital momentum more effectively if given some significant blocks of time (meaning about 30 seconds at a time) in between "stirring bursts." When the reaction is clearly starting to get vigorous and hot, crank the stirring to 10 and leave it on. NOTE: This is where you can take advantage of Mr. A's trial and error regarding this reaction's parameters. If you used the kind of foil specified, prepared it as specified, used no more than the specified 400mg HgCl2, and used a 2-liter and NOT a smaller flask, you can breathe easy knowing that the reaction is going to hum along nicely but will not get out of control, and will result in perfectly processed aluminum amalgam sludge. You may think that a 2-liter flask is oversized for this reaction, but that is precisely the point. The extra headroom in the glass provides a nice zone of "breathing room" for the reaction and facilitates good refluxing. I've seen this reaction get out of hand in a 1000mL flask, and it isn't pretty, believe me. Use the 2-liter. 11. As the reaction progresses only a few minutes after the addition was started, you will observe that the aluminum is breaking up fairly rapidly. This is good, as long as you have the ketone/nitro mixture dripping in at a good rate of about 2 drops per second. But be careful with the addition rate at this point, as a rate that is much faster than this could easily send the reaction into overdrive (not good). Your reflux should be unnervingly vigorous as the amalgamation really starts to pick up speed, with the MeOH dripping really fast down out of the condenser. I know it's hard to believe, but this is what you want, this is good. I'm telling you, LOTS of trial and error came before this writeup. Trust me. You will also see sludge already starting to settle at the bottom and forming a ring on the glass around the top surface of the spinning mess. The consistency will get thicker by the minute. Add more ice to your bucket as needed. 12. At this point you can sort of control the reaction rate by slowing down or speeding up the addition rate a bit. Of course the reaction is already barreling along, so you won't want to speed it up much. The concept here is that you want the addition of the ketone/nitromethane to be paced neck-and-neck, as it were, with the breakdown of the foil as it amalgamates and gets turned into sludge. In other words, you have to watch those two things and sort of adjust the addition so that they proceed at approximately the same rate. It's tricky, and imprecise, but with a little experience and intuition you'll get the hang of it. Sure, you could be lazy and just leave the addition at a steady 2 drops per second the whole time, but if the amalgamation peters out way before your addition is finished, and you find yourself adding your beautiful ketone to impotent sludge, don't cry to me. The addition should take about 40-45 minutes in total, and as it's finishing, the state of the aluminum should be about 95% broken down. In fact the reaction should by now (~45 minutes after addition was started) look like a really thick, steely-gray chowder with only minor small slivers of undissolved aluminum visible if any at all. You will probably even need to add an extra 20-30mL of MeOH down the condenser at this point (or before) to help it keep stirring effectively. This is no problem. A note about color at this point is helpful too. Comparing successful reactions to failed ones, I have observed that there is a distinctive color to the mixture early on that indicates healthy amalgamation and foretells a successful run. At a point maybe 30 minutes or so post-addition, the reaction takes on a color that I would describe as being "light steely gray with blue overtones." It is a hard thing to describe shades of gray, but I will try. It is a light shade, akin to the color of common gray sweat pants, but like I say with a very slight suggestion of a blue hue in there as well. This is in contrast to what I saw in failures resulting from using too thick of aluminum and not enough HgCl2, where a dark metallic gray with definite green overtones (from unreacted ketone) was noted. NOTE: Another point I would like to make about the timing of the addition against the breakdown of the aluminum is that Mr. A found that there was a definite "spike" curve to the amalgamation reaction which was easily observed by watching the reflux rate. That is to say, there is a peak that it builds up to and then comes down from. At this scale, and using the exact materials described herein, that buildup to peak and subsequent slowdown occurs over approximately 25 minutes or so---very fast. So at only about 20-25 minutes after you first started feeling the amalgamation heating up, it will have slowed to a reflux of about 2 drops per second, after having been at a peak with a reflux rate so furious it is a stream, not drops. At one hour and 15 minutes after you first started the addition, the reflux will have slowed to a very calm 1 drop per 2 seconds or so. Finally, when... A) the reflux has slowed to almost no reflux at all B) if you stop the stirring you do not see any small bubbles anymore C) no "uneaten" aluminum is visible and the solution is a thick, uniform gray soup, ...the reaction has essentially finished. It will reach this state at about one hour 45 minutes to two hours after addition was started. Nevertheless, you will leave it stirring happily for a total of three hours after the addition was finished to assure that the reaction has run its full course and the conversions that you desire have had ample time to take place. In fact you should add a bit of external heat at the point where the addition has finished and the reflux slows down dramatically, because I've found that if one doesn't, there might be a bit of aluminum that refuses to break down all the way which results in the later extraction being messier and much more of a hassle. One reason I bring this all up is that there has been lots of talk about how this reaction needs 8 hours or 24 hours or even 36 hours to run! But those time frames apply only in cases where much thicker aluminum is used, and/or in variations using methylamine and not nitromethane. Mr. A was never successful in using thicker aluminum, and doesn't want to be! Why would someone want to make a reaction take any more time than it needs? Beats me! I'm mystified! The approach illustrated in this writeup optimizes this reaction to finish in 3 hours 45 minutes from beginning to end, and it probably doesn't even need that much time. 13. If you chose to apply external heat, turn it off at about 30 minutes before the targeted finish time. Otherwise you will have to wait an extra 30 minutes (at least) for it to cool for the next steps. 14. When finish time has arrived, dismantle your setup, set aside your reaction flask, and make 750 mL of a 35% NaOH solution (750 mL H2O + 262.5g NaOH) and let it cool to room temp or below (safety glasses!). 15. Into a separatory funnel no smaller than 2000mL capacity, pour your beautiful gray reaction mixture, being very careful to KEEP THE STIRBAR FROM FALLING IN to the sep funnel and breaking it (that would be ugly). If your mixture is really thick, you may need to add small amounts of MeOH to thin it to a pourable consistency. This is perfectly fine. Wash the final residue out of the reaction flask with a few mLs of MeOH and add it to the funnel also. 16. Slowly pour the NaOH solution into the sep funnel (gloves and glasses! no excuses!). That's right, don't dump it in wholesale. Basifying should be a gentle process. If you bully those molecules they may decide they're being disrespected and choose not to cooperate. Adding the NaOH will cause the mixture to warm up a bit as the very last bits of the aluminum are dissolved, which is fine. Swirl it a couple times and give it about 10 minutes to cool down to something closer to ambient temperature. That yummy stinky methylamine smell tells you that the reaction was successful. 17. When the mixture in the sep funnel has cooled down, extract it once with 400mL toluene followed by once with 100mL toluene. These are the critical moments for your yield now, so you be sure to shake long and hard (at least 3 minutes) during these extractions (I don't have to tell you to vent do I?!). The toluene/product layer will of course be on top since toluene floats on water. Also, be sure to give the separations ample time to happen (at least 15 minutes); it is easy to tell when it's okay to separate because the interface of small toluene bubbles finally resolves and you have a nice clean line between the layers. If you like, do as Mr. A does and finish off with a final small extraction of 50-60 mL toluene just to get the last of the stuff. NOTE: Your extractions will contain a tiny amount of the base/metal/garbage from the bottom layer; this is inevitable but easily worked around in this way: when you have collected your combined toluene/product extractions in a bottle, chill that bottle in the freezer for 30 minutes or so. When cold, the garbage gets a lot less mobile and it is easy to decant the toluene away from it. Just be vigilant while pouring the last 50 mL or so and avoid letting that glob of crap rejoin the toluene. Yeah, you will lose the very last 2 or 3 mL, but that's life. Alternatively, you could filter it through a paper towel, but you will still lose the same amount when the towel absorbs it. Just get over it and move on! 18. If you haven't already, drain the garbage layer out of your sep funnel into a storage bottle or something, and wash the garbage residue out your sep funnel with water. 19. Wash the toluene/product 4 times (or more) in your sep funnel with 400 or 500mL H2O and a final time with 500mL of a saturated NaCl solution to remove any traces of solvated HgCl2. 20. Dry your toluene/product solution with 30g of your favorite drying agent (MgSO4 recommended) in an acetone-cleaned, heat-dried bottle for no less than 45 minutes (Mr. A is superstitious so he lets it sit for an hour). Shake it a few times during this period. 21. Filter the solution and gas it with that good ol' HCl bubbler setup. Be smart and use just enough muriatic (31% HCl) to wet the salt but not enough to make any puddles, and put a wad of drying agent wrapped in tissue paper in line somehow between the reaction flask and the tube leading to your pipette end. Weep with joy as a bumper crop of white precipitate crashes out of solution. Expected yield: approximately 20-21.5g raw odoriferous product that will purify via careful recrystallization to 17-18g of beautiful snow-white MDMA! Ain't life grand? ~~~"There's a methyl to my madness"~~~  ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~
	ikb3 (Stranger) 07-09-00 15:32 No 26780		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			Thank you for the timely response. However, I am even more confused, but I do not feel bad since I suppose that even those that know something about chemestry could be confused. First, I am looking at a one Oz. bottle of Sassafras Oil distributed by Now Foods, and it says right on the label: "Sassafras Oil 100% pure!" (emphasis added!!!) Secondly,I appreciate your thorough knowledge concerning these matters -- one reason I asked you the question rather than someone else -- however, you did not "thouroughly" explain that part of my question. You thoroughly exlained the Safrol purification process. Therefore, if Sassafras is the same thing as Safrol, why all the fuss, especially if one thinks he or she has 100% Sassafras, hence Safrol? Or am I to understand that since What I am looking at is 100% Sassafras therefore it has no Safrol? I hope that this does not further annoy you, but I would appreciate a bit of patience of you. Again Thanks, ikb3
	Rhodium (Chief Bee) 07-09-00 15:49 No 26785		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			What they mean by 100% sassafras oil is that it contains nothing else than the oil gotten from sassafras roots. This oil contains in turn 75-90% safrole depending on source. http://rhodium.lycaeum.org/
	LaBTop (Moderator) 07-09-00 15:54 No 26787		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			But it's not anoyment, it's amazement. You have 100% Safrole in hand, but better don't believe them, that's where all the shit starts, you better check with TLC (Thin Layer Chromatography, an expensive looking bag of words, but in fact a quite simple technique, you can master, it safes you many mistakes), if they really did allready the distillation process for you. If you get only one distinct spot on your TLC plate, then kiss the bride, if not, start distilling. TLC : see thread nr.2 up in the forumlist from the Newbee forum, and look it up, it's there, the whole explanation. Never believe a Food supplier firm, they are no professional chem suppliers, and they could mingle with the figures.. they mean that they didn't spit in it, when they say "pure", but you can not compare their terminology with that of real chemistry firms, who are bound to standard rules. LT/ PS: It probably is what they say, 100% pure Sassafras oil, however, that's not pure Safrole, it will contain mostly safrole plus a few other aromatic oils, so a healthy first-buy portion of mistrust can't hurt, ain't it ? WISDOMwillWIN
	ikb3 (Stranger) 07-09-00 16:41 No 26799		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			thanks for the help: I can't seem to find the post in question. Would you please be more specific. (Where is TLC described in detail on the above threads) thanks Ikb3
	ikb3 (Stranger) 07-09-00 17:56 No 26815		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			My problem is not being able to read your post, but finding the thread you write about! I have gone to Newbee forum and then I went to the numbers listed on bottom page (are these the threads?) and I can not find the topic. I went to the "Search" and the only listing of TLC is what you wrote in this thread and several other insignificant posts. thanks again ikb3
	LaBTop (Moderator) 07-09-00 18:34 No 26829		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			English not your language? Either is mine, but I understand when someone tells me to look for the 2nd thread in a forum. [url]Cat=&Board=newbee&Number=26266&page=0&view=collapsed&sb=5&part=&vc=1" target="_new">http://hive.lycaeum.org/wwwthreads/perl/showflat.pl? Cat=&Board=newbee&Number=26266&page=0&view=collapsed&sb=5&part=&vc=1[/url] CHEMISTRY LINKS COMPILATION , study it, come back in august as an enlightened new member. Look there for these sites, one of them has a good description of the technique, with "comics" WizardX website Worlocks website The Village idiots website And here is much more of it too : http://hive.lycaeum.org/cgi-bin/ubb_cgi/Ultimate.cgi?action=intro The Hive Archives, search for : TLC as the subject. WISDOMwillWIN
	Semtex (Newbee) 07-10-00 21:59 No 27366		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			LT, good post, you have KOH mentioned in the text of the isomerization but not in the chemicals list. At least on this new software you can edit rather than having to repost...  Thanks for the most detailed write up yet...  When can we look forward to seeing the "IVa" writeup...? "Chemicals: 15.5-17.2 L purified safrole oil >98% pure. 1 kg Aliquatt336 (Methyl-tri-octyl-ammonium-chloride) ~>98% pure, from Merck or Fisher etc. 3 kg Florisil (=magnesium silicate=CAS 1343-88-0 )~>98% pure. 5 L DiChlorMethane ~>98% pure. 1 kg pack of silicagel beads 2-5 mm from Merck, Fisher etc.; or 1 kg MgSO4.7H2O industrial grade. 5 L Silicone oil from Shell, Exxon etc. Tapwater (H2O) from your government, and lots of ice cubes or blocks ."
	ikb3 (Stranger) 07-10-00 22:52 No 27384		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			thank you for taking the time out and making the access that easy. I've been busy going through those resources and I must say that it is reminiscent of a kid in a candy store! However, curiosity got the best of me and I must ask you a question. I understand direct proportionality in chemistry, as well as in other things in life, but why use such large quantities in the "methods for non chemists" post? I mean you are talking about  16L-18L of Safrol, etc. Again, thanks and I'll be in touch in August!
	LaBTop (Moderator) 07-11-00 18:38 No 27707		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			Because you can scale them down, but also infinitely UP ! I also gave the quantities in grams in at least one synth, but take your calculator and multiply all figures by XXX, or divide them by XXX. At least all my methods, Beaker stated that his method doesn't scale up more than ~50 gram, and I bet you that he/she tried more grams. LT/ FUCK FUCK FUCK, just had a FUCKIN MAJOR EARTHQUAKE here. Many walls in my house are ripped, lucky it did not go down. Learns you some dignity and respect for "Mother Gaya"  !!! Shit, it's still wobling, better go outside again. Had to login via another ISP, the other one is down and out, will be a lot of damage everywhere. Is now 10 min ago. A shocked LT/ WISDOMwillWIN
	Semtex (Newbee) 07-11-00 18:42 No 27711		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			A very wise man once said that if one were to choose a certain profession, that one should make as much as one could in as short a time as possible and get out of the biz...  Try and take into consideration, hindsight IS usually 20-20...
	Beaker (Stranger) 07-11-00 21:11 No 27756		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			"At least all my methods, Beaker stated that his method doesn't scale up more than ~50 gram, and I bet you that he/she tried more grams." No I didn't(exactly), and no I haven't. But, perhaps I was not clear in exactly what I meant. What I literally meant is that 50g is about the max you could reasonably process in one batch in a 2L flask. Scaleup should not be a problem, but due to the rather low product loading that you can obtain with the method as written, it is rather impractical at >50g scale. Bigger than that and I would suggest that one look into catalytic hydrogenation a la KrZ's mescaline writeup or finding a way to cut the amount of solvent back quite a bit. For most people, ~80g of 2CB out of 100g, or $60 worth of 2,5-dimethoxybenzaldehyde is more than enough. However, since you have gotten this impression, I will correct my lack of clarity in the original thread.
	CHEMMAN (Hive Bee) 07-12-00 03:42 No 27878		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			Good your back LT. Ive just learnt a lot by mixed successes and fuckups . Yep the big ways are what we want hahaha. Keep up the good work, and next time I mightnt have to learn the hard way..:)
	LaBTop (Stranger) 07-12-00 03:42 No 23325		Detailed Methods for Non-chemists Edit: IT'sDONE!	Bookmark Reply
			DETAILED METHODS for NON-CHEMISTS              ============================ LIST of SYNTHESIS (red list-text = method new/altered) : I.------Sassafras rootbark -or- (chemical synthesis)--> SAFROLE. II.-----SAFROLE--> IsoSAFROLE--> MDP2P ketone--> MDMA , MDA, MDEA. III.----Lowpressure Catalitic Reduction--> P2P ketone--> METHAMPHETAMINE, (METH, ICE). IVa.----2,5-Dimethoxybenzaldehyde + PTC (PhaseTransferCatalist)--> Nitrostyrene--> 2C-H (2,5-DMPEA , 2,5-dimethoxyphenethylamine)--> 2C-B and many more highly interesting unexplored 2C-(X) analogs, -or- IVb.----MESCALINE--> MESCALINE Nitrostyrene--> 2C-H--> 2C-B etc. V.------2C-B a la Lycaeum. VI.-----AMPHETAMINE PRECURSORS CLEANING/WORKUP.( The Cure) VII.----EPHEDRINE to METHAMPHETAMINE + RP/I2. VIII.---SIMPLE HCl GASSING/BUBBLING APPARATUS. IX.-----NITROMETHANE --> MDMA. X.------FORMALINE + NH4CL --> METHYLAMINE.HCL XI.-----DMF O2 WACKER. XII.----MDP2P + NMF --> MDA ( Leuckart big scale) XIII.---Bright Star's MDMA synthese. XIV.----Rhodium's SAFROLE to ISOSAFROLE routes. XV.-----LaBTop's d- and l-isomerisation procedures ------------------------------------------------------------------ METHODS : I.------Basic-Extraction -or- Supercritical-Extraction--> Steam-Destillation. II.-----Fractional destillation--> Aliquatt336+KOH (a la Osmium)--> Classic Performic (a la Ritter)--> Al/Hg (a la Osmium) -or- NaBH4 reductive amination (a la LaBTop) -or- lowpressure reduction (a la KrZ). III.----Lowpressure hydrogenation (a la KrZ)--> Destillation--> Reductive Amination NaBH4 (a la LaBTop) -or- low pressure technique (a la KrZ). IVa.----Addition + PhaseTransferCatalist (a la Rhodium and Beaker)--> Lowpressure Catalitic Nitrostyrene Reduction (a la KrZ) or Beaker's synthesis--> --> Addition (a la Shulgin). Or 2C-B synthese a la Lycaeum, -or- IVb.----Supercritical-extraction -or- (chemical synthesis)--> Nitrostyrene synthesis (a la Rhodium)--> Electrochemical Reduction (a la Uncle Fester)--> Addition (a la Shulgin). V.------2C-B a la Lycaeum.(Andrew Edmond) VI.-----AMPHETAMINE PRECURSORS CLEANING/WORKUP : The Cure (Placebo) VII.----EPHEDRINE to METHAMPHETAMINE + RP/I2. (Placebo) VIII.---SIMPLE HCl GASSING/BUBBLING APPARATUS. (Psychokitty) IX.-----NITROMETHANE --> MDMA.(Methyl Man) X.------FORMALINE + NH4CL --> METHYLAMINE.HCL. (Vogel) XI.-----DMF O2 WACKER. (Strike, KrZ, Grouch) XII.----MDP2P + NMF --> MDA. ( Leuckart small/big scale, LT/) XIII.---Bright Star's MDMA synthese. XIV.----Rhodium's SAFROLE to ISOSAFROLE routes. XV.-----LaBTop's d- and l-isomerisation procedures **And anything else found economical interesting for the creative home brewer** ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ METHODS merits : First of all : Dr. Alexander Shulgin : No need for words, the greatest ! Paul Nels Rylander : for his extensive work on practical hydrogenation techniques. Hat off ! Strike : For creating this place, and giving a wealth of information in her books. A big hug ! (Still did not received your books, how come?). Eleusis : For starting a really interesting discussion in the early days of this board, ultimately costing him his freedom. The Lycaeum : For sheltering this place for so long allready, against mainstream US policy, and not interfering with our freedom of speach. Rhodium, for collecting all that priceless information on his website, the best there is for the underground chemist or cook. Secondly: Overall methods : Rhodium, Osmium, Rev drone, Labrat, Cesium, Spiceboy, Ritter, Beagle boy, KCN, Station, Sunlight, Sumerian, Gyrogearloose, iudexk, Ymir, Methyl Man, Psychokitty, Chem_Guy, Bankrobber(and some more, fill them in later). Hydrogenation : KrZ (mainly !), Rylander, pHas3d, Titanium, Equarius (and some more, I fill them in later). Electrochemical Reduction : Uncle Fester (mainly !), Dwarfer, Worlock, WizardX etc. O2 Wackers : KrZ, Strike, Bright Star, Grouch, and more will follow ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ =================================================================== SAFROLE: Materials : Same as for IsoSafrole. Chemicals: 16-18 L non purified safrole oil 70-90% pure. 20 L industrial Silicone oil or Peanut oil for oil-heatingbath. +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Method : S1. - First you have to clean your safrole oil by fractional distillation. S2. - This means that you separate different fractions of your impure reagens fluid (safrole here), those fractions will have different boiling points. That way you split the impurities from your desired oil. S3. -You start heating up your impure Safrole and let it first come to a steady constant boil at the first temp where this will happen, under your vacuum, reached by your vacuum pump; keep the temp at that point until no more fluid comes over in the collecting flask, put that aside after releasing the vacuum, put the cleaned/dried collecting flask on again, and put vacuum on again, and then slowly incline the temp until boiling starts again, repeat as many times that you reach different boiling temps (at least 5 C apart from eachother). S4. - You will at a certain temp (here ~ 130-145 C , depends on the strength of your vacuum), get the biggest fraction, which is safrole, and the other fractions will be only very small. These other fractions can be used ~ 5x again in next batches (see below at S8.). S5. - If you use a 22 Liter 3-neck flask for it, and you don't have a big magnetic stirrer, you must use boiling chips in it, about 1 % oil-volume procent, so for a ~3/4 filling = ~16-18 liter filling (never use more then ~3/4, or fluid, not vapour, will boil into your condenser) you need 160-180 ml chips roughly (~). S6. - Measure them in a measured beaker in ml volumes, don't worry about the loose spaces between them. S7. - If you use a magnetic stirrer bar ( MUCH better!) and an aluminium pan as an oilbath, filled with peanut- or silicone oil, so you can use the stirrer, because the pan is from aluminium ( stirring strong and big enough), then there is no need for boiling chips, they would even damage the flask in one run. They would work as a grinding machine on the innerside of the glass flask, together with the big magnetic stirbar; or if you use a overhead stirrer, like a variable speed drill, or a non-sparking induction electro-motor; together with the stirrer propellor. S8. - Any for-or after-run(s) at a temp more then 5 degrees C different from your main safrole body, you must throw back in the next 16-18 L safrole batch you start up after some day(s). After 5x doing this, you throw both away, it's more rubbish then safrole by then. You re-use these fractions 5x because they allways will still contain some pure safrole oil. S9. - Pure safrole oil is light yellow and smells a bit sharper sweet then the ketone, MDP2P (MethyleneDioxyPhenyl-2-Propanone), which has a much softer sweeter smell and is a bit more yellow then the pure safrole; if you work perfect, the pure safrole and the pure ketone will have no color at all, and the ketone will be a bit more syruppy (thicker) then the safrole. S10. - Safrole can be fractionally distilled at ~130-140 C temp using a new refridgerator pump(as your vac source, 1/8 horsepower, buy them from a fridge repair shop, $120) or a normal oil-filled vacuum-pump or much better: use allways a diafragm-vacuumpump, no oil which can and will be contaminated every time you use a oil filled pump, so it looses its vacuum-power; and standard glass distillation setup with a 40-60 cm icewater cooled fractionating/reflux-condenser and using a 22 L roundbottom flask hanging in an oilbath filled with peanut oil or better silicone oil as an egally heating source, and a big collecting flask. S11. - Under the aluminium oilbath you would use a magnetic stirrer/heating plate with enough electrical power/watt's. Don't let the 22 L flask touch the bottom of the aluminium pan, keep it ~1 cm above the bottom, to prevent extreme hot-spots which could decompose your safrole or ketone. S12. - Grounded standard glass-connections/fittings should allways be used on your distilling glassware. S13. - Cold circulating water for the condenser comes via 2 tubes (one hanging loose at the water level in the icewater bucket) from an aquarium water-pump (expensive ones 70-80 dollars, cheap ones 10-20 dollars), submersed in a styrofoam isolated bucket or drum filled with ice cubes in water, which you re-new from time to time. S14. - Distillation generally takes 4-5 hours depending on size, and heat applied. Always a good idea to insulate the fractionating column, and 22 L flask-neck with the condenser/refluxer on it; with heavy duty aluminum foil. Just wrap it around all the glass parts. Make ~1 cm2 holes, 5 cm apart from each other, in the aluminium wrapping then, to see what happens inside the glass parts. S15. - The main safrole oil body (ca. 15.5-17.2 L), which boils (at~ ~130 C) and comes over at your vacuum ( should be 20 mbar or lower), you collect to proceed to make: =========================================================================== ISOSAFROLE (Aliquatt336/KOH method) : Materials : 1--Magnetic stirrer/heating combi plate + minimal 1 big magnetic eggshaped stirrerbar, to use in roundbottom flasks, and 1 straight one, for flatbottom flasks. or: 1--Kg boiling chips. (Pumis-stones, crushed raw flowerpot pieces, crushed raw porcelaine, cat-litter). and : 1--22 L round-bottom, 3-neck, glass vacuum-flask with 3 standard grounded neck- fittings. 1--portion High-vacuum silicone-grease (Merck f.e.), to thinly grease all grounded glass-fittings, allways both male and female grounds. 1--Still head, to connect one of the grounded necks of the 22 L flask to the grounded inlet of the condenser. 1--40 to 60 cm glass condenser, preferably the one you see with ~ 8-12 glassballs blown inside ( for use as reflux condenser). 1--big enough (min. 5-10 liter) collecting glass-flask with standard grounded fitting. 1--Vacuum glass-alonge with male and female standard grounded fittings and vacuum-tube fitting. 1--Vacuum tubing, 3 meter long, shorten it to the minimal length from alonge to pump, must fit tight on the alonge and the vacuum pump. The shorter, the better the vacuum. The remaining part you use for your aspirator vacuum, you will use it for volatile solvents removal/recovery. 1--Water driven PTF, Nylon or PVC vacuum aspirator, connected to a water tap with sufficient pressure and cold enough water, to use in case of electrical power failure and for evaporating low boiling vapours, f.e. methanol, acetone, dichloromethane etc. Never use an oil-filled vacuumpump to do that. A diafragmpump can do it, but why should you take the risk of damage to your expensive pump, when you can use a $40 aspirator for simple solvents evaporation ? 1--Big thinwalled flatbottomed aluminium pan, to fit the 22 L flask in. Buy it at a chinese restaurants supplier-shop. 2--Glass or digital thermometers, -30 to+300 C, one to use in oilbath or icebath and one in the flask-neck, long enough to reach the fluid inside. The best would be to have another one with small grounded glassfitting in a 2-neck Claisen type still-head setup between the 22 L flask and the condenser, to measure vapour temps. This is not directly necessairy, but is handy to see if the vapour temp suddenly varies, that means you have to put vacuum off and collect that last fraction, because the next fraction is coming. 1--10 L jerrycan with peanut oil or better silicone oil (the big oil-company brands suppliers have it, such as Exxon, Shell, Mobil). 4--Big lab-stands with 8 lab-clamps to rig up your distillation setup. 1--Big bucket or drum, isolated with styrofoam or insulation blankets used in building industry, to use as ice-water circulating tank for the reflux/condenser. 1--Aquarium or fish-pond water-submersable circulation pump in that bucket or tank.. 1--5 meter long water tubing, cut in half to fit the condenser and the watertap or circulating pump. 1--Multiple (6) electrical connections box with main ON/OFF switch. Panic : all electricity OFF. 1--Fire-extinguiser, for those unlucky moments. CO2 or special chemical-gas filled one. Better not a powder filled one, you will find out why, when you have to clean that stuff. 1--Drying oven, up to 350 C. old household-one sufficient enough, preferable electric. Gas burning type gives off water vapour and an open flame is not safe in a lab environment. 1--10 L filter flask, heavy walled, with vacuum side-adapter fitting. With some creativity you can use a big thickwalled glass Chianty wine bottle with a 2 hole stopper, one hole for the Buchnerfilter and one for the vacuum. 1--5 Liter (~) PTF or PP or PE or PVC or porcelaine or glass Buchnerfunnel. 1--Set of commercially sold rubber V-shaped rubbers in different sizes, for Buchner and to fit in mouth of filterflask. 1--Pack of round filterpapers, to fit nearly exact in the Buchner filter funnel. Attach the filterflask fitting to the tapwater-aspirator-vacuum pump for a safe vacuum. 1--~20 L clear plastic carboy used in drinking water utilities : ( to use as a self constructed separator-funnel : cut a 5 cm hole in the center of the bottom to use as filling opening, which you can close later with a 5 cm rubber stopper, so must be nice round, and push firmly a big rubber stopper with a center hole, in the excisting mouth at the top of the carboy. Fix the stopper with iron wire, so it can never plop out, or safer, use any clamp which fits the mouth of the carboy and covers the stopper ~half. Push a tight fitting glasspipe, with a glass-valve attached to it with a small piece of silicone-tubing which tubing you strap with those nylon straps used in car-repairshops, into the stopper, not extending above the other end of the stopper. Voila !) 4--25-30 Liter PTF or PPP or PE plastic jerrycans, cleaned and dried. 1--Box of heavy duty Reynolds wrapping aluminium . 1--Big steady lab table with a vinyl, or the like, coating. 2--Comfortable chairs, to sit in during those long waiting hours. 1--Small TV with antenna. Less entertainment-greedy persons can help themselfs with a ghettoblaster radio/tape-recorder/CD-player. 1--Pile of Playboy's, Hustler etc. or a big vibrator, also very handy to separate layers in your home-made separator funnel ! Just keep it tight against it. Must be ON then. It vibrates the oil out of the fluids ! Chemicals: 15.5-17.2 L purified safrole oil >98% pure. 5.611 kg KOH flakes (~98%, industrial grade). 1 kg Aliquatt336 (Methyl-tri-octyl-ammonium-chloride) ~>98% pure, from Merck or Fisher etc. 3 kg Florisil (=magnesium silicate=CAS 1343-88-0 )~>98% pure. 5 L DiChlorMethane ~>98% pure. 1 kg pack of silicagel beads 2-5 mm from Merck, Fisher etc.; or 1 kg MgSO4.7H2O industrial grade. 5 L Silicone oil from Shell, Exxon etc. Tapwater (H2O) from your government, and lots of ice cubes or blocks . +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Method : I1. - If you have any doubt that your now pure Safrole oil is not dry, so has some water in it, first dry it by shaking or mixing in your 22 L flask (or a suitable 20 L jerrycan) with a stopper in all necks at least 1 hour with 5% weight/weight silicagel beads or MgSO4.7H2O which are both first dried in an oven for 3 hours at 250 C. Then decant(in case of silicagel) or filter the MgSO4 off and proceed as soon as possible. Your oil MUST BE DRY ! I2. - If you must filter MgSO4 off, then use the big Buchner filter with a round filter paper in it, pre-wet the paper with some oil, push all airbubbles away formed under it, and carefully decant your oil/MgSO4 mix in the middle of your filterpaper, better use a big spoon laying in the middle of your paper to pour slowly in, so you don't disturb the fixation of the filterpaper, until at least a 2 cm layer is reached, now put your aspirator vacuum on, attached to the 10 L vacuumflask, take the spoon out, then you can proceed somewhat faster decanting while the vacuum sucks much faster then mother earth's G-force. The MgSO4 stays behind on the filterpaper. Don't leave any MgSO4 in the container, swirl from the beginning to have it good mixed with the fluid. Otherwise you have a truckload of MgSO4 left in the container, wetted with Safrole, and how do you get that out then ? I3. - Pour 10 kgmoles safrole oil ( ~16.219 kg) in an open 22 L flask, only a thermometer immersed in the fluid, add carefully 12 kgmoles KOH flakes (~5.611 kg) via a widemouth plastic funnel (the solution will immediately turn black.brown): crush the KOH to not too small particles, ~1-2 cm, first, f.e. in a thickwalled plastic bag with a big hammer, ONLY if they are really big. Normally you don't need to do this! Don't get carried away by your enthousiasm and slam it, just push, be carefull, KOH in your eyes is not pleasant at all. Don't crush it too small, you must be able to decant or filter the oil later easily. I4. - Stir for 10 minutes with the magnetic stirrbar or overhead stirrer , the solution will warm up allready caused by some exothermic effect, nearly no KOH will dissolve, which is no problem at all and is normal. That's why there may be NO water in this stage of the reaction ! Or the KOH will dilute in the water and can not be filtered off later, and more washing steps are then needed. I5. - Keep stirring and add 5 kgmol% pure PTC (PhaseTransferCatalyst)= here Aliquatt336 (~811 gram), and everything will 'seem' to slightly change color and take a slight shift in viscosity. When adding aliquat, the aliquat will float on top until the temperature rises,then it mixes all up into one fase. I6. - Now commence heating/stirring and read your thermometer in the fluid, after ~ one hour it will reach 80 C , keep the heat at 80 C for only 5 minutes, then the heat must be shut off totally, then allow the fluid to stir until roomtemperature is reached again. Don't forcefully cool with icewater or so. This will take ~2 hours. I7. -After cooling to room temperature, the mixture is poured out of the flask into a 25-30 L jerrycan, trying to keep as much KOH flakes in the flask as you can without loosing too much oil, wash the flakes with 250 ml DCM and add that to the IsoSafrole allready poured out, and then you dilute the decanted IsoSafrole with 5 L DCM (DiChloroMethane), shake thoroughly, and pour out and filter that mixture over 1 Kg Florisil (=magnesium silicate=CAS 1343-88-0 ) in 3x equal portions, the second and third time renewing the Florisil again (1Kg) in your Buchnerfilter setup. Just scrape the old, used Florisil away with the big spoon, a littlebit left on the filterpaper will do no harm at all. Try to not move the filterpaper, and wet it a bit with a spoonfull new oilmix again, before you pour the next 1 Kg portion Florisil in the funnel. So remember : you need 3 Kg Florisil , filter in 3 portions of 1 Kg. I8. -Wash then all Florisil, collected together, with 333 ml DCM 3x, so 1 Liter DCM totall, and add that DCM, after you let the Florisil precipitate, to the main IsoSafrol/DCM mix. If it is cloudy with some Florisil , use a new filterpaper in the Buchner funnel, and pour those 750 ml DCM with the washed out IsoSafrole in it through the filter into the main mixture. I9. -You now have a mix of pure IsoSafrole and DCM in the vacuum flask, which you have to pour out 3x into a normal, for chemical storage used, 25 L plastic polyphenyl PTF or polyethylene PE jerrycan. I10. -DCM is then removed at ~60 C oilbath-temp under reduced pressure from your water-aspirator in your 22L destillation setup. I11. -You now have pure isomerised olefin, IsoSafrole, purity ~>96 %, left in your destillation flask and recovered also your again pure DCM from your collector flask (change the flask several times) to use again. I12. -[THIS STEP IS ONLY NEEDED WHEN THE pH IS TOO HIGH -or- YOU THINK THERE IS STILL TOO MUCH WATER LEFT IN THE ISOSAFROLE]. Check the pH of the pure IsoSafrole with a pre-waterwetted pH paper, and if it is extensively higher then pH 11 , that means there is still too much KOH in the oil, which quickly will decompose the oil when you have to store it, so then you wash it 1x with 1 L water to get rid of any KOH, which will dissolve in the water part. In a big 20 L carboy separator funnel, fill the IsoSafrole and the 1 Liter water, shake as hell, and separate the water on top of the oil then as carefully as you can, so no water will stay in the oil. Test then if the pH of the IsoSafrole is not too high, should not exceed 11.5 . Now you add 5% in weight, dried silicagel to this still littlebitt water holding IsoSafrole oil, to remove all traces of water. Shake 10 minutes and then decant the oil or leave it in until you proceed with the next step and then decant in your clean 22 L destillation flask or whatever you use in that step first. I13. -You proceed with this IsoSafrole to make : =========================================================================== MDP2P : MethyleneDioxyPhenyl-2-Propanone (Classic Performic acid method) : ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ Isosafrole --> MDP2P via Modified Classic Performic Acid : Materials : Same as for ISOSAFROLE, plus : 1--minimum 500 liter stainless steel milk coolingtank, with a big-ass cooling coil in the double walls, preferable in the bottom also. 1--Mixer motor, 220 Volt, non-sparking, induction type, for : 1--Mixer propellor + axle (diam. 1.5 to 2 cm), stainless steel, diam. 40 to 60 cm. 1-- 100 liter plastic container to prepare the PerAcid mix. and/or : 1--big-ass 80 liter dripping funnel, stainless steel, plastic or glass. Homemade is cheap. 1--1 meter cooled refluxing column, glass or stainless steel, to fix on the only opening of the milktank which is left open to the air. 5--meter heating cable, chemicals resistant, to use in milktank for the hydrolisis step with 15 % H2SO4. Chemicals : Reaction : 27 kg IsoSafrole, purity >/= 96 %. 99.7 kg DiChloroEthane, ClCH2CH2Cl, Industrial quality >/= 98 %. or : 99.7 kg DiChloroMethane, CH2CL2, Industrial quality >/= 98 %. 8.3 kg SodiumBiCarbonate, NaHCO3, pure. 41.5 kg Formic Acid, HCOOH, 86 %. 25.1 kg HydrogenPeroxide, H2O2 30 %. 22.43 kg Sulfuric Acid, H2SO4 Industrial quality ~99 %. 127.07 kg water, H2O, pure. 42.4 kg Methanol, CH3OH, Industrial quality >/= 98 %. Extraction : To extract from 218,9 kg hydrolized Glycol/15%H2SO4/CH3OH mix : 60 liter DCM or DCE = 3 x 20 liter, Industrial quality >/= 98 %. Method : Here are the original figures from literature in grams, for a 27 KG batch of Iso-safrole to MDP2P : ---(all figures multiplied with: 27000 grams devided by 16.25 grams = multiply them with 1661.54 ) --- M1. - Combine 16.25 grams [or 27 kg ] of Isosafrole with 50 ml=60 gram (1 liter DCE or DCM = 1,2 kg), [or 99.7 kg] DCE (DiChloroEthane) or DCM (Dichloromethane) plus 5 Grams [or 8.3 kg] Sodium bicarbonate (Sodium Hydrogen Carbonate : NaHCO3). Can be made by bubbling CO2 gas in a strong soda solution (Na2CO3.10H2O ), the sparsely soluable NaHCO3 will precipitate. M2. - Let it vigorously stirr for 2 or 3 hours, depending on the strength of your mixer [a total of 135 kg ]. This gives it time to form a pH-buffering complex which facilitates the next reaction enormously. M3. - Seperately s.l.o.w.l.y combine (under external cooling) 25 gram [41.5 kg] 86% Formic acid and 15.1 grams [25.1 kg] 30% fresh Hydrogen Peroxide (to create Performic acid) and cool to 0 C. Note : It is critical to cool when preparing this mixture or else it will, after sitting for 3 or 4 hrs without cooling, start boiling and nasty fumes will fill your lab and you will have to evacuate the place. M4. - Then drip this cold Performic-acid [66.6 kg] VERY VERY slowly , into the 135 kg ISO-DCE-Sodiumbicarbonate mix, keeping temp under 40 C with external ice-bath or other means of cooling until all is in , CO2 bubbles out of the reaction mix while dripping in (and watch the temp for the following 1-2 hours, after completing dripping in, closely, so it still can not exceed 40 C). M5. - Stir !VIGOROUSLY!, preferably with an overhead stirrer, for a total of 6(six) hours. M6. - Stop stirring and move the whole batch in portions to a big seperatory funnel, and let it sit for one hour in there. M7. - It will be orange-juice color DCE/pre-MDP2P(Glycol) mix at the bottom and clearish performic acid mix (H2O2/HCOOH) on top, the orange layer with the pre-MDP2P (Glycol) and DCE is heavy, so it goes fairly fast to the bottom of the funnel. M8. - Important Note: --------------------------------------Many members have reported a switch of layers when they used DCM. Iso/DCM layer on top OR at bottom ! There is a perfectly logical explanation for this phenomenon : The one's who's cooling equipment functioned o.k. and thus kept the temperature between 36-40 Celsius will see the Glycol/DCM at the bottom after separation period, because they still have all their DCM left in the mix. The one's who were not so lucky and let the temperature get out of hand will see the orange layer at the top, due to an extensive loss of DCM which evaporated into thin air. The densities of the normal Glycol/DCM mix and the PerAcid mix lay close together, so if you evaporate too much DCM this balance is switched and suddenly the PerAcid mix is the heaviest layer, and falls to the bottom. You will notice then a light yellowish PerAcid mix at the bottom and a orange-juice coloured Glycol/DCM mix on top. This is no reason for real worry, unless you boiled most of the DCM away (not good for your health if you were in the same room (carcinogenic) AND not good for the reaction which did not have enough cooling capacity anymore in the last stage, depending on how high you overshoot the temp. Boiling temp of DCE = 83 C, DCM = 40 C , that's the reason WHY you must keep the temp under 40 C when you use DCM! And you must also do this when you use DCE ! Instructions are allways given with a reason, which is in literature expected to be common knowledge, but not here at a forum crowded with C(r)ooks (hehe) and a few real chemists. Thought I owed the Cooks the explanation for this reason. ------------------------------------------------------------------ M9. - Seperate into a new empty container and evaporate (low-vacuumdistillation, but KEEP the TEMP under 60 C!! so use more vacuum , so go lower then 700 mbar if the temp rises too high) the DCE off and stock that recovered DCE for future use. M10. - You should add now 180 grams [but in reality, in contradiction to the official reference, only HALF the amount necessairy!, so 90 grams = 149,5 kg] of 15% Sulfuric acid (H2SO4) [so : add 22.43 kg 99% H2SO4 to 127.07 kg water], boil it until it starts refluxing back with slight addition of 60ml=51 gram Methanol [only HALF! needed, so 25.5 gram = 42.4 kg Methanol (1L methanol=0.85 kg)] through the cooling/reflux condenser added on the distillation kettle for 2 hrs. No longer then 2 hours !!! Or you will begin to loose product-yield. You now converted the Glycol to raw MDP2P, mixed with some pollutants. M11. - Let it cool and extract 3 times with enough DCM (or DCE), (minimum 10 reactionvolume-percent per extraction). M12. - Combine the DCM or DCE extractions and then boil the solvent (DCM or DCE) off (in fact no vacuum needed, but if you are in a hurry:)with one or more aspirators combined or diafragm vacuumpump to get brown oil that is peppery and cardamon smell. M13. - You get around 16 grams [26.6 kg] -dirty- MDP2P. M14. - To get the real clean MDP2P, you will have to vacuum-distillate this dirty MDP2P-base again to get a reasonable yield of about 73-75 % (grammole-percent)= 17.8 kg clean MDP2P which should be light yellow, or if you distill exact and have no leaks to let tiny amounts of air in, and you don't let the temp go over 170 C, at ~20 mbar vacuum, it would be clear with no color. ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ Note: In weight/weight procents you get 16 / (16.25 / 100%) = 98.46 w/w % , but yield is scientifically allways given in Mole-percents, so: (16 gram x 178.188=molecularweight MDP2P / (16.25 gram x 162.188=molweight Iso / 100%) = 2851.008 grammole / (2635.555 grammole / 100%) = 108.17 mole %. But the effective mole % after distillation (=ultimate clean-up, no washings then necessary!) is 75%. 20 mbar x 0.01450138 = 0.29 psi, which is good enough for all distillations we work with ! ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ Here are the four threads on the old board I found back again which are relevant for the classic performic: 1. Post No 107771 LaBTOP-Gyro performic results - Sumerian . 2. Post No 107780 LaBTop-Gyro's Modified Performic Questions - Synthia. 3. Post No 107770 New Performic Scale Up Question - artech. 4. Post No 107739 The correct way to mdp2p via performic - gyrogearloose . And this is the original Classic Performic post in the thread : http://hive.lycaeum.org/ubb_board/Forum3/HTML/000613-3.htmlNaBH4 question : solution: One Pot ! : Classical Per-acid oxidation of Isosafrole to get Piperonylacetone (MDP2P): (Iso.) [R]-CH=CH-CH3 ----> [R]-CH2-C(=O)-CH3 (Pip.Ac.) R=Methylenedioxyphenyl The PerAcid solution is made from 25 g. HCOOH (formic acid)(86% ,starting from 99% HCOOH) and 15.1 g. 30% H2O2 (hydrogen peroxide). This sol. is added to a mixed sol. of 16.25 g. Isosafrole(>/=90%) and 1,5 g. NaHCO3 (!!) in 50 ml CH2Cl-CH2Cl at 35-40 C. The temp. is during 6 Hrs. mixing regularaly checked and kept within 35-40 C. The solvent is evaporated (vacuum, keep TEMP! UNDER! 60 C.!). Residue is boiled with 180 g. 15% H2SO4 for 2 Hrs. Extraction with 3 x 100 ml.CHCl3, wash with water,dry over MgSO4 and evaporation of the solvent gives a brown oil (purity >/=90%). Supplemental purifying by Kughelruhr destillation (~70 C, 0,2 Torr) gives 70-75% yield of MDP2P (>/= 95% pure!) ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ And this is the latest info from Ritter, who by the way posted this method first, then Beagle_boy , then me, then Gyrogearloose, so this method needed 3 times posting to get the attention needed, so lets call it from now on the Classic Performic, to avoid any misunderstandings: Ritter (Stranger) 06-20-00 14:26 Re: LabTop modified performic method? The reaction runs best as described in my writeup! Adding carbonate to formic/peroxide first would surely lead to a nasty volcano and would not help any. Carbon Dioxide is emitted as performic is slowly added to alkene/carbonate solution. As far as advances are concerned a few things have been realized. Extremely vigourous stirring, such as that produced by a mechanical stirring rig, seems to increase yields. If a considerable amount of isoalkene is recovered during vacuum distillation an easy solution is to add more performic acid mix to rxn. This is usually an indicator that the peroxide used has degraded somewhat below 30%. With this MDP2P you proceed to make : ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ NaBH4 : REDUCTIVE AMINATION of MDP2P and P2P : ------------------------------------------------------------------- REACTION MECHANISMS :               H               |    H   H   CH3 C2    \ /   /             //  \    C N    //    \  / \ / \ O--C3      C1   C   H    H2C/   |       ||   |\       \   |       || H3C H O--C4      C6            \\    / \             \\  /   H C5       |               H . . .                     C11H15NO2 . .     3,4-METHYLENEDIOXY-N-METHAMPHETAMINE . .                      EXTASY . . .       O       v     O    CH2CCH3    / \ //\ / H2C   |  ||      +  H2NCH3  -- Methanol ->    \ / \\/     O . . MDP-2-P    + Methylamine gas in Methanol -> . . . .       NCH3       v     O    CH2CCH3    __> Extract with Silicagel    / \ //\ /   / H2C   |  ||      + H2O --- NaBH4 --->    \ / \\/     O . . IMINE + adsorped Water   --- add boro ---> . . . .       NHCH3       |     O    CH2CHCH3    / \ //\ / H2C   |  ||    \ / \\/     O . . 3,4-METHYLENEDIOXY-N-METHAMPHETAMINE NOTE : We know now, july 2000 , that it's much better to follow the basic rules from the P2P to Methamphetamine synthesis also for the MDMA and MDA synthesis, in fact you MUST use silicagel (pre-dried at 300 C for 2 hrs) in all relevant steps, especially, when you make first the imine and later the amine conversion by adding NaBH4 to the Imine. MDP2P/Methanol/Methylamine mixing converts already to the Imine plus water, so you add silicagel to obtain the perfect results, for both MDA and MDMA and also for Methamphetamine. So keep this in mind when you read the following texts. The imine is formed when you mix MDP2P with 10% w/w MeNH2 / MeOH,( so then allready you must have added the 20% w/w pre-dried silicagel beads, to directly take up the water formed by the imine reaction mechanism), not when you crystalize, mixing acetone, that you do with the pure distillated freebase. No imine left there. The imine is hydrolized with the flooding with 8x water (ev. mixed with 5% NaOH or KOH, as Sunlight happily found out for the MDA One Pot ammoniumacetate and NH3 gas route ). You see a picture of the total mechanism into the MDA route, with molecular drawing of the imine, right above here, many seem not to know what the exact mechanism is, it will help you out. If you make the acetone/HCl mix in advance for the crystalisation of your destillated clean amine-base, you must use it as soon as you can, or it will even become red, depending on how much HCl you bubble in. And add the acetone/HCl mix then slowly to the MDA (or MDMA or MDEA or Meth)-freebase while medium stirring, not the other way round, that would lead to decomposition when you start adding a part of your base, due to too acidic conditions. It has been seen that vigorous stirring results in very fine crystals ; medium and at the end slow stirring results in more voluminous crystals, which is a logical effect of giving the crystals time and a more undisturbed medium to grow together. The best is to keep your percentage of HCl fairly low, to avoid early decomposition. ------------------------------------------------------------------ MDP2P--> MDA : Materials : Still looking for the best yield possible, using basicly the description of the Methamphetamine ICE OnePot synthese (see below) and some minor or major changes, so you change only P2P to MDP2P and Methylamine to Ammoniumacetate or NH3 gas, see the ongoing discussions in the Methods forum for all possible improvements. Changing the solvent, Methanol, to Glycol,  and Ammoniumacetate to Hydroxylamine f.e. could do the trick, research is going on. Chemicals : The indicated route to MDA with Ammoniumacetate below will result in no more then between 30 and 60% yield for less experienced members, so for the time being you have to live with that, or improve yields by following the basic rules from the Methamphetamine One Pot. Work with ANHYDROUS Ammoniumacetate, and dry all steps with Silicagel or MgSO4 or Na2SO4. ------------------------------------------------------------------ Method : To simplify life for you all, here's the ULTIMATE FOOLPROOF EASIEST WAY to make: MDMA, MDA, MDEA (use ethylamine instead of methylamine) if you have the chems available! A practical way to make Honey (tinted bases) is as follows:   Parts |  M D A -base || Parts |    M D M A -base    0,5 |  MDP2P (oil) || 1,0 |    MDP2P    3,0 |  MeOH (solvent) || 3,0 |    MeOH    1,0 |  A.Acetate (salt) || 0,3 |    MeNH2(gas)    0,1 |  NaBH4(reductor) || 0,1 |    NaBH4 These quantity-parts are in weight! So: you can choose if you want to work in gram OR kg. Following starting quantity is 25 kg MDP2P or ev. gram, but then you must divide all other quantities by 1000, so kg's and/or liters ): Prepare 6x20 L yerrycans in wich you can fill each 12,5 L cooled, (-20 C) MeOH. In each yerrycan you dissolve 1,25 kg methylamine in the cooled MeOH (methanol).Let the MethylAmine dissolve in the -20 C cooled MeOH which you already put in the freezer one night before! Use a upside down laying gastank with MA (30-45' angle)and fill with a thick synthetic black rubber hose the liquid-MA as deep as possible in the MeOH. SLOWLY! It takes ca. 10 min., per yerrycan. The yerrycan stands on a digital balance, so you know the weight added. Surround the hose with a wet towel at the filling opening of the yerrycan for the unhealthy smell. When ready fill all the yerrycans with the MeOH/MeNH2 mix in the reactiontank. [Add in case of (MDA) now the AAcetate (in the pure methanol) instead of the MeNH2 gas !]. Cool now the reactiontank to +5 C and start the mixer anticlockwise, so the fluid circulates from bottom to top. This way no air is mixed in, so less oxidation. Add at +5 C the 25 L. MDP2P .(pre-cooled). Start then directly (because a slow reaction starts already), every ca. 5 min, addition of the NaBH4, ca. 3 soupspoons per time. Use a funnel and wash every time with a little methanol. Keep all holes closed inbetween or it stinks! Because of the excessive cooling the temp. will not rise much, only to +15 C. Wait again till ca. +7 C to add again. Are you impatient and add to quick, then the mix will start heating, evenso boiling! This may never occur,then your product will be lost ! This process takes ca. 7 hours. Ending temp. will be ca. 25 C. Stop after 7 hrs. the cooling and let react with mixer on for 29 hours. After this time, you prepare 200 L clean water, which you mix with 10 Kg NaOH or KOH, until all is dissolved. This 5% water/NaOH-mix you add to the cooling tank (fast), then you measure the pH, should be between 11,5 and 12. (If you add coincidently acid instead of NaOH base, greenish fat form in and on the fluid). Stop after 10 min. the mixer and let the raw brown base precipitate 30 min to the bottom and tap off the base through the valve at the bottom. Stop tapping when you see lighter color (water) coming. Add now 3 liter methylenechloride (dichloromethane=CH2Cl2) to the tank, mix 10 min., stop the mixer, wait again 30 min. and tap off the rest of the base, now diluted in the CH2Cl2.This gives totally ca. 43 L raw base. Now we remove the CH2Cl2, Methanol and the water in a simple distillation setup, with low vacuum circa 500 mbar, with magnetic mixer/heater, mixerpin teflon, glassware with NS29 connections ( 20 L 2-neck flatbottom flask PYREX!, thermometer, cooler 60 cm, glas-alonge and 10 L collecting flat-bottom erlenmeyer flask). Start at 35->55 C for CH2Cl2, then 55->85 C for methanol and 130 C for all the water. Re-use the CH2Cl2 and the methanol! Now you are left with ca 28 L half-clean MDA or MDMA amine-base (depending on the fact if you used Am.acetate or MeNH2 gas, colour is light brown).Now we will clean the raw base by 2 times recrystallisation with acetone 98%, (m)ethanol 98%, and after that washing min. 3 times with acetone 98%. Use 20 L P.P. plastic buckets to do this. Mix 5 L base (cold) and 10 L icecold acetone. Leaf inductionmotor-mixer on. Bubble HCl-gas 99% through with 1 meter StainlessSteel pipe, (inner diameter min 5-8 mm) until white crystals form. Stop when pH= 7,0 and start with the next 5 L base. The first one will rise again to ca. pH=8,0. Later you can bubble again a littlebit HCl-gas through until again pH=7.0 or even to pH 5.0 . Let the crystals precipitate and pour the upper acetone off. Re-dissolve the wet crystals now in the minimum quantity of HOT(nearly boiling) methanol or ethanol in a metal bucket (because its hot !) until you see no more crystals, so you now have a saturated solution in (m)ethanol! Pour 5 L of this solution back in the plastic bucket, and add 5 L Acetone, which is -15 C. When cooling down, you will see crystals form again,in a dirty solution. Wait until no more crystals come, pour off again and dissolve again in hot (m)ethanol. Do this as many times until you have snowwhite crystals. Dry on glasplates on the floor with blower. You now have H(M)ONEY in the Bank. ------------------------------------------------------------------- MDP2P--> MDMA Another write-up. Materials : idem Chemicals : idem ------------------------------------------------------------------- Method : ------------------------------------------------------------------- Preparation of MDMA by reductive amination with sodium borohydride by Labtop (written by Quicksilver, editted by LaBTop) ------------------------------------------------------------------- - Introduction Until recently reductive amination with NaBH4, for the production of MDMA, was assumed to be inferior to the well-known NaCNBH4 route (that has been popularized by Alexander Shulgin for the production of MDA) and other synthetic routes, like aluminum amalgam. The following method proves that the NaBH4 reduction actually is superior to all other common routes used in clandestine chemistry. The method is relatively simple, it doesn't require complicated equipment. The work-up on the reaction mixture is simple and efficient. The method is very usefull for big scale production of MDMA and gives high yields (+90%!). There is a relatively rapid formation of the imine and the imine is reduced relatively rapidly. There's no reduction of the ketone to the secundary alcohol, as one might expect(2). In similar reactions, the water!! that is produced during the forming of the imine (Schiff Base) is removed from the reaction before the imine is reduced. As we know now,much better with pre-dried (3 hrs in oven, 300 Celsius) Silicagel beads, 3-5 mm diameter, take a quantity of 20% weight compared to your MDP2P weight. Because of the stability of the imine, this is not necessary for the production of MDMA, but should in fact allways been done, to reach maximum yields ! This reaction is an improvement of a known synthesis (1), a similar reduction in an aqueous sollution of ethanol was performed, but the yields were only 31%. - Synthesis : MDP-2-P + methylamine-> intermediate imine +H2O-> MDMA freebase-> MDMA HCl salt. - Ingredients MDP-2-P 1000 g Methanol 3000 g (>99%) MeNH2 (gas) 300 g (99,9%) (Be very carefull with MeNH2-gas: it is toxic and carcinogen, but when handled with care, no problems. I advice to not use a gasmask, because when you smell it, you can avoid it, but with mask you are not warned and it can be uptaken through your skin! Use wet towels to avoid problems at ev. leaking points!). NaBH4 100 g . (NaBH4 is a common reducing agent. Do not spill NaBH4 on hands or face without noticing it(e.g. whiping sweat off your face), or you will be punished with red spots there which will never go away! It takes minutes before you feel the pain, and then its too late. So wash face and hands with water, frequently.). filtered clean H2O. 33% HCl . conc.NaOH solution . DCM (DiChloroMethane). Acetone >98%. - Equipment : *-- There are several options for the reaction vessel. One could think of a 500 to 1500 L stainless steel milk cooling tank, that is modified to ones needs. But a fermentation tank (plastic or stainlees steel, from 20 to 8000L), with small modifications will do just as fine. Or one could buy a 1m3 (=1000 L.) plastic tank everywhere at second hand tank and cans stores. Have a handy manhole to clean, are totally airtight and as a bonus, have a nice tap-valve at the bottom.They ship NaOH ,33% HCl etc. all over the world with them. *-- A solid diaphragm vac.pump is recommended for the vac. distillation. For example a Vacuubrand Type MD 4C, 3.0 m3/h. It sucks from 1.7 to 11.2 m3/hour, ask for Chemistry Design(PTFE) series. *-- MeNH2-gas is made by reacting MeNH2.HCl with conc.NaOH. (An other option is to react 40% MeNH2 with dry KOH.) (I will add a lot more on MeNH2 synthesis shortly.) - Step by step : 1) Preparation : Dissolve 300 gram, not ml ! methylaminegas in chilled 3000 gram methanol (-20 C). Cool in the mean time the reaction-mixture to +5 Celsius. Start the mixer (anticlockwise so no air is mixed in) and add the 1000 gram MDP-2-P. NOTES: Make 300 gram MeNH2-gas by reacting MeNH2.HCl with NaOH. Or dissolve the methylaminegas at hand from a gas cylinder in methanol, using an upside down laying (45 degree's) gascylinder with (fluid) methylaminegas in it, no pressure regulator on it. Attach a thick black synthetic rubber hose to the valve, open that valve slowly ,while the hose is down at the bottom of your first jerrycan with icecold Methanol, which stands on a big flat digital balance. Surround the hose with a wet towel. Add slowly 300 gram gas in the jerrycan. Be aware of a popping sound when the gas implodes when it enters the Methanol. Don't let suck back, close the valve everytime suddenly. 2) Reaction : Start adding NaBH4, one teaspoon ca. every 5 minutes, H2-gas bubbling has to disappear before adding again, temp. should be between 8-18 deg C. (Wash down with methanol). Adding of the white NaBH4 powder will take 7 hours. With mixer on let it sit for 29 hours more.(4 hours will do for people that are in a hurry,loss 20-30% yield). NOTES: When the reaction vessel is opened it should be covered by a wet towel, so the methylamine-gas can be absorped by the water. (1 L water absorps 1000 L NH3.) An airlock might be sufficient for that goal too. Do not airtight the flask, let a thin tubing out the window,wrapped at the end with a WET towel! 3) Work-up I : Leave the mixer on. Add 8 L clean H2O with 1%=80 mL 33% HCl. (The 80 mL HCL is redundant, don't add it at all!). (When making MDA as your endproduct, you add 5 weight % NaOH or KOH to the water, to facilitate a good separation in the following separation procedure). Liquid will be greenish brown, pH=10,5 (11,5 is better than 10). !!When green soap possibly starts to form: you made a mistake, you added far too much HCl ( To avoid any risk: do not add it at all. Redundant!!)... Brown freebase will sink to the bottom of the vessel. Tap off, till a bit clear water is coming out of the valve. Close then the valve. Add 200 mL DCM to the reactionvessel and mix for 10 min. Stop the mixer and wait 30 minutes. The DCM with the rest of the freebase will sink to the bottom. Tap off. Combine the two. There will be app. 1750 mL of base fluid + DCM. NOTES: You can again basify the water with conc NaOH sol. to pH =13-14 and tap off the last oil. The 8 mL 33% HCL (1%) is added to the water to make sure any unreacted NaBH4 is neutralised, but is not needed, in the following steps this is taken care of automatically. 4) Work-up II : A vac.distillation setup is prepared. First the methanol, DCM, water and other lowboiling stuff are removed, then at 165 C the clean freebase comes over. Approx. 1.0 L. freebase. NOTES: Step 1. The water and other lowboiling stuff comes over at 130 C. Remove when nothing more comes! Step 2. Set on 165 C. At first around 140-145 C you see the first little drops of clear oil condensate and at 160-165 C and 20-18 mbar it starts Running! To distill of the water, methanol and other low boiling stuff from the reaction mixture, the use of an aspirator is sufficient! To get the freebase out, the use of a decent vacuum pump is recommended. 5) Crystallization : Mix the base 1:4 with clean,cold(-10 to -20 C) acetone and bubble through with a Stainless steel pipe 8 mm x 1 meter with HCl-gas 99%. SLOWLY! After ca. 5 min a thick, white crystal mass will form. Check frequently with pH-meter ( aquarium shops sell good ones from Hanna Instruments for circa US$ 60.- ), or pH papers from Merck, until pH = 7 to 5 . If the mix get too hot, place back in big freezer to cool and proceed with next cold batch. Be very carefull not to go under pH=7 to 5, because then your powder will solute again and you must add base again until pH comes up again to 7. So keep always at least 20 mL freebase ready in case of mistakes ! Dry the acetone/powder mix in a Buechner-funnel with aspirator vacuum. Dry again on glassplates on the floor under airconditioner or slow blowing fan's in a dry room. - Epilogue : There are reasons to believe that the salt form of the amine can be used, ( I don't think it will be interesting, without high decrease of yields LT/ 10-07-2000) but the gas method is by far preferrible. Ethylamine can be used to produce MDEA. Ethylamine is a gas above 17 C, but a fluid under 17 Celsius, so very convenient when first placed in a freezer,  just pour it in the icecold methanol then. Ammonium acetate or NH3 gas to produce MDA is another possibility, Sunlight and Cesium have researched the Ammonium Acetate process further and reached yields of ~ 50-65 %. The same method was tried with P-2-P, first with unsatisfactory results when NO !! water was removed, because the imine that's formed here isn't as stable as the MDMA or MDA imine. When you remove the water while forming,with a drying agent, Silicagel, this also works (12-07-2000) perfectly, even better !!! Quantitatif yield near 100%. - References 1. Noggle, F. T.. Jr., DeRuiter, J., and Long, M. J.. "Spectrophotometric and Liquid Chromatographic identification of 3,4-Methylenedioxyphenylisopropyl-amine and its N-Methyl and N-Ethyl Homologs." Journal of the Association of Official Analytical Chemists, Vol. 69. No. 4. 1986, pp. 681-686. 2. Shellenberg. K. A.. "The Synthesis of Secondary and Tertiary Amines by Borohydride Reduction." Journal of Organic Chemistry, Vol. 28, Nov. 1963 pp. 3259-3261. 3. J. Weichet, J. Hodorova and L. Blaha, "Reductive amination of phenylacetyl-carbinols by sodium borohydride." Coll. Czech. Chem. Commun. 26, 2040-2044 - CA 56, 5864c (1962) ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ MDP2P--> MDEA : Materials : Same as for MDMA. Chemicals : Same as for MDMA, except : 1.--- A equimolar amount of Kg Ethylamine, CH3CH2NH2, compared to the amount of Methylamine in above One Pot's. A gas at +17 C, a fluid gas under that temperature ! ------------------------------------------------------------------- Method : Same as for MDMA. Only switch methylamine gas for ethylamine gas or fluid-gas. ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~
	LOONYTOON (Newbee) 07-13-00 01:51 No 28253		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			Thank You Thank You Thank You THANK YOU This is exactely the kind of information i've been looking for. For some reason everyone assumes that just because you want to learn how to make drugs you either have to get a phd or you'll kill yourself. Everyone assumed i just wanted to be told how to it step by step, when all i really wanted to know is what i have to know and what i don't have to know, you know? I just didn't want to pour over tombs of knowledge that have nothing to do with what i want to learn, at least until i can find the time to do so. But i didn't want to go about it blind either. You gave me exactely the kind of shortcut i needed, which really isn't a shortcut at all, just cutting through all the bs. Stupid people have it easy. (I made that up, aren't i clever? Don't answer that)
	sunlight (Newbee) 07-13-00 05:40 No 28318		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			LabTop, in the cryystalliztion mehod, you mix the amine with acetone, may be MDMA difficultly form the imine with acetone, but with MDA it seems easier, so we are afraid this crystallization method can yield imine. HCl instead of amine HCl, what's your opinion ? does it work sure ? Recently we have tested bubbling HCL in acetone before, as you told time ago, using the acid acetone soon, it degrades quickly to a yellow/green solution froming some kind of chloro subproduct, and we found this very volatile (as we supposed) and very very toxic and nasty. We didn't like it, although it's a good option.
	Shambhala (Stranger) 07-13-00 08:39 No 28357		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			hank You Thank You Thank You THANK YOU                     This is exactely the kind of information i've been looking for. For some reason everyone                     assumes that just because you want to learn how to make drugs you either have to                     get a phd or you'll kill yourself. Everyone assumed i just wanted to be told how to it                     step by step, when all i really wanted to know is what i have to know and what i don't                     have to know, you know? I just didn't want to pour over tombs of knowledge that                     have nothing to do with what i want to learn, at least until i can find the time to do                     so. But i didn't want to go about it blind either. You gave me exactely the kind of                     shortcut i needed, which really isn't a shortcut at all, just cutting through all the bs.                     Stupid people have it easy. (I made that up, aren't i clever? Don't answer that) Who has that WTF happy face?  I don't think this thread should be filled with ________ posts (fill your descriptive word for the above post on the line).
	LOONYTOON (Newbee) 07-13-00 18:12 No 28521		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			You know what? After reading your post a little more thouroughly, i think i overestimated this info at first glance. If this is supposed to be for non-chemists, then you must have something against them. Pretend for a second you have no knowledge of chemistry. Then read your post. Stupid people have it easy. (I made that up, aren't i clever? Don't answer that)
	LaBTop (Moderator) 07-14-00 12:00 No 28797		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			Don't start ANY chemistry then, you will fail. If you can't understand chewed out proposals like these, then you better start a career as a barber, having the advantage that you see a lot of people (a cook does/must not), and you can talk a lot, to amuse your customers. Think about it, it's a good, solid profession ( This all must be taken lightly, btw, did I tell you that I hate tags? ). LT/ PS: posts like the above even more hardened my desire to write-for-the-masses, what a relief, one less to worry about. PS2: Au contraire, this post is exactly meant to post all replies in, the original locked sticky thread is at the Newbee forum at the top. It gets periodically updated and cleaned from all barbershop-talk. PS3: Nevertheless, thanks for the first enthousiastic response, but it shows (in your own words later) that thoroughly reading is not a barbers strongest point. Behold, no harm done, it's even an advantage for that trade. Never saw a barbershop blow up, never read about it either, must be a safe haven from the malice of modern society. hehehehe arrrr fuckin hilarious reaction arrrh... PS4: By far not ready yet, next one is Methylman's synth, that should be an easy one for analfabetes. PS5: If you feel in any way harassed by these words, save your breath, I probably saved your life and/or freedom, and gave you some solid free advice for a thrilling career, nearly forgot that. (All advice given in a modestly hilarious mood btw.) WISDOMwillWIN
	LaBTop (Moderator) 07-14-00 14:29 No 28867		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			The imine is formed when you mix MDP2P with 10% w/w MeNH2 / MeOH,Edit 15/07( so then allready you must have added the 20% w/w pre-dried silicagel beads, to directly take up the water formed by the imine reaction mechanism)End Edit not when you crystalize, mixing acetone, that you do with the pure distillated base. No imine left there. The imine is hydrolized with the flooding with water (ev. mixed with 5% NaOH or KOH, as you happily found out for the MDA One Pot route. I will fill in a picture of the total mechanism soon into the MDA route, with molecular drawing of the imine, many seem not to know what the exact mechanism is, I'll help you out. Yep, if you make the acetone/HCl mix in advance, you must use it as soon as you can, or it will even become red, depending on how much HCl you bubble in. Edit 15/07 And add the acetone/HCl mix then slowly to the MDA (or MDMA or MDEA or Meth)-base while medium stirring, not the other way round, that would decompose at the start a part of your base, due to too acidic conditions. It has been seen that vigorous stirring results in very fine crystals, medium and at the end slow stirring results in more voluminous crystals, which is a logical effect of giving the crystals time and a more undisturbed medium to grow together. End Edit The best is to keep your percentage of HCl fairly low, to avoid early decomposition. LT/ WISDOMwillWIN
	zooligan (Hive Bee) 07-24-00 10:19 No 32604		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			Never saw a barbershop blow up, never read about it either, must be a safe haven from the malice of modern society. From http://www.thesmokinggun.com/archive/albertan1.html "Back in 1957, crime boss Albert Anastasia was gunned down as he got a shave in the barber shop of New York's Park Sheraton hotel. The murder of the bloodthirsty Anastasia, who was alternately known as the "Mad Hatter" and "Lord High Executioner" of Murder Incorporated, was never solved. Here's a selection of documents from the official investigative files on the Anastasia killing."
	LaBTop (Moderator) 07-28-00 09:41 No 34234		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			Repaired it myself, thanks. LT/ WISDOMwillWIN
	sunlight (Hive Bee) 08-25-00 01:28 No 45035		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			LabTop, our first test with am acetate and NaBH4 yielded 50 % +, but next tests have produced low yields, 25 - 30 %, and it is not a problem with the work-up as we thought the first time with low yields. Finally we realized that our first test was done with conservative proportions of am. acetate-ketone, using the amounts of TSII, and by the way, we don't remember the amount of NaBH4. It should be studied better, our experience is that using your proportions yields are around 30 %. Even using your exact recipe for MDMA, usual yields are 78-80 %, and adding a 20 % more of NaBH4 (may be a 10 % could be enough) yields are 84-88 %. It's what we have seen.
	LaBTop (Daddy) 02-05-01 11:57 No 171287		Re: Detailed Methods for Non-chemists . edit 6feb1	Bookmark Reply
			METHYLAMINE.HCl salt production. Ultraman (Member)01-30-00 00:27 No 123283 Questions about MeAm formation Concerning H20 + Paraformaldehyde + Ammonium Chloride -> MeAm.HCL: 1. Is ALL MeAm produced during the 4-5 hour reaction period ? i.e. Is the reaction complete at this point ? 2. Is the rest of the distillation work after this 4-5 hour period just for seperation of the MeAm from the reaction by-products ? 3. If 2 is correct, then could one bypass further distillation and proceed directly to refluxing the contents of reaction flask in denatured alcohol to dissolve the MeAm and Buchner filter out Am.Cl. crystals, repeating several times until all Am.Cl. has been removed ? 4. Assuming that 1 and 2 are true, if the MeAm and Ammon.Cl. solution is left sitting in the flask after the 4-5 hour reaction period (say for a period of 48 hours), will the reaction reverse itself ? Will any other product formation occur ? LaBTop (Moderator)01-30-00 14:08 No 123284 First, read ChemHacks long posts about the procedure, Do you see the light allready after reading ChemHack? Now follow Sploofer's advice and go to a Uni library and ask for Vogel's Textbook of Practical Organic Chemistry. Read all about Methylamine Hydrochloride(from formalin) under Aliphatic Compounds. You will see now that you use technical formaldehyde solution (formalin, 35-40 per cent. formaldehyde), AND not PARAFORMALDEHYDE (anhydrous!), which you only use to make trimethylamine,HCl at 160 C. Dimethylamine you make at 115 C. Methylamine you make at 104 C and you mix 2 parts by weight of formalin(ca. 35 % formaldehyde) with 1 part by weight of ammoniumchloride. The method in Vogel is one page long in small typesetting. If you do it that way, you can't go wrong. READ IT! 250 g Ammoniumchloride(NH4Cl) + 500 g formalin 35-40% (HCHO) gives 100 g Methylamine,HCL. (CH3NH2,HCl) Answers: 1.Yes, you can stop when no distilate is collected anymore. 2. No, it is a lot of recrystalisations to get the highest possible yield. AND to separate the ammonium chloride and the dimethylamine,HCl and the methyl formate and the methylal from the desired Methylamine,HCl. 3. No. 4. A lot of other product formation. You wanna watch TV inbetween? Some sexfilm? Tsktskstsk...  LT/ Ultraman (Member)01-31-00 02:35 No 123285 sexfilms?? naaa, not me. Savin my bones for glassware  .... besides, too busy looking out the window for cops. LaBTop: I've searched the hell out of the hive and it seems as if most references indicate that Paraformaldehyde is de-polymeramizable (is that a word)- add to water to depolymerize it, and is usually dissolved by the time the solution reaches 55-60°C. Have I been mis-informed ? 1. Werner in the JCS 844('18) 2. Sigma Product Information Sheet P.S. I'd lock up that old copy of Vogels you got - seems to be priceless from what I've researched so far. The current edition doesn't mention a damn thing about MeAm recipes, or many other goodies. LaBTop (Moderator) 01-31-00 05:21 No 123286 paraFormaldehyde can be seen f.e. as 3(HCHO)3 , a chain of formaldehyde molecules. If you add water and warm it up, the chain will break up again into separate HCHO molecules, and you have formaline again. So tell me, why you want to buy the more expensive para form, when you gonna mix it with water again? Quite unlogical thinking. Formaline 35% (rest is water) is shit cheap. Ok, just insured my Vogel for 10,000$, and am now typing the recipe out for you. In the mean time, say as loud as you can : Thank You, LT, 1000 times. LT/ LaBTop (Moderator) 01-31-00 06:23 No 123287 Vogel :  Methylamine Hydrochloride (from Formalin) Place 250 g. of ammonium chloride and 500 g. of technical formaldehyde solution (formalin, 35-40% formaldehyde) in a 1-litre distilling flask : insert a thermometer dipping well into the liquid and attach a condenser for downward distillation. Heat the flask on a wire gauze or in an air bath slowly until the temperature reaches 104 degrees and maintain the temperature at this point until no more distillate is collected (4-5 hours) (note 1). Cool the contents of the flask rapidly to room temperature and filter off the ammonium chloride (ca. 62 g.) which separates rapidly, at the pump. Concentrate the filtrate to one half of the original volume on a water bath, when more ammonium chloride (ca. 19 g.) will crystallize out on cooling to room temperature. After filtration at the pump, evaporate on a water bath, until a crystalline scum forms on the surface of the hot solution. Allow to cool and filter off the methylamine hydrochloride (about 96 g.) (note 2). Concentrate again on a water bath and thus obtain a second crop (about 18 g.) of methylamine hydrochloride. Evaporate the mother liquid as far as possible on a water bath and leave it in a vacuum dissicator over sodium hydroxide pellets for 24 hours ; digest the semi solid residue with chloroform ( to remove the dimethylamine hydrochloride), filter off (note 2) the methylamine hydrochloride (about 20 g.) at the pump and wash it with a little chloroform. [ Upon concentrating the chloroform solution to about half the original bulk, about 27 g. of dimethylamine hydrochloride may be obtained : the mother liquor should be discarded.]. Purify the crude methylamine hydrochloride by placing it together with 250 ml. of absolute alcohol in a 500 ml. round-bottomed flask fitted with a reflux condenser carrying a cotton wool (or calcium chloride) guard tube. Heat the mixture to boiling for about half an hour, allow the undissolved material to settle and decant the clear solution. Cool the solution when pure methylamine hydrochloride will separate : filter (note 2) and use the filtrate for another extraction. Four or five extractions are required to extract all the methylamine hydrochloride. The yield of recrystallized material is about 100 g. Notes. (1) The distillate weights about 110 g. and contains methyl formate and methylal. If it is placed in a flask provided with a reflux condenser and a solution of 25 g. of sodium hydroxide in 40 ml. water is added, the methyl formate is hydrolysed to sodium formate and the methylal separates on the surface. The latter may be removed, dried with anhydrous calcium chloride and distilled : about 30 g. of methylal, b.p. 37-42 degrees, are obtained. If the aqueous layer is evaporated to dryness, about 25 g. of sodium formate are isolated. (2) The best method of drying the precipitate of methylamine hydrochloride is by centrifuging ( see it rev drone, that's why a centrifuge is handy in the lab ) ; the compound is hygroscopic. -Vogel end- Ultraman (Member) 01-31-00 10:04 No 123288 x 1000, hell make that  x 2000. Would you mind scanning the whole novel and placing it out on the web somewhere ? If you don't mind too much, back to a modification of my original question.... If formation of MeAm is complete after the 4-5 reaction period, then I assume it doesn't matter if you vac distill at this point to concentrate solution. There seems to be different opinions/techniques about applying vac after the reaction period around the hive. Seems if reaction is complete after 4-5 hours, then why not use vac to concentrate... it would just speed up the process, and keep temperatures down. Is there a disadvantage to it ? Product loss perhaps ? Thanks a mill LaBTop. LaBTop (Moderator) 01-31-00 14:31 No 123289 I have a feeling that good old Birdie would have had the same idea, but ended up with a lot of bunk when he vacuumdistilled the whole batch after 4-5 hours, so he choosed for this method. If your still curious, devide all quantities by 10 and try it out. Could work, with perhaps only a small loss of yield, but practice will teach the truth. LT/ LaBTop (Moderator) 01-31-00 14:44 No 123290 Oh yeah, the centrifuging has of course the advantage that it can be done in a few minutes, while evapping off in open air or a open distillation system will turn your MeNH4 into a watery sludge. You use a linen sack in a vedgetable centrifuge or something like that, the more speed, the drier. LT/ ChemHack (Member) 01-31-00 14:52 No 123291 The reason to use paraformaldehyde is if you can get it at the hardware store and the only formalin you can get without going to the chem supply shop is full of blue dye and purfume for portapotty use. Paraformaldehyde justs lets you stay that much farther under the radar. Depends on the level of police control in your state. Best way to deal with paraformaldehyde is not to dissolve it in water because that takes way too long. Instead to dissolve it in concentrated (much stronger than from grocery store) ammonium hydroxide (blue printing solution) to make a solution of hexamine in water. Then evap away some of the water and add Hydrodchloric Acid and procede from there. The HCl breaks the hexamine back into formaldehyde and ammonia. The ammonia reacts with the HCl to make ammonium chloride and you are right where you wanna be to start the rxn. Heat to 104C and go. LaBTop (Moderator) 01-31-00 15:12 No 123292 Thanks, chemhack, good additional info. In europe, you just say that you need the formaline for your hobby of preparation of dead animals you found along the highways. In fact you use the para-form to rub on the inside of the skins, and the formaline to put them in glas jars. LT/ Ultraman (Member) 01-31-00 19:01 No 123293 Ok, just one more question about technique. See a lot a references (hive, Vogel, and elsewhere) using Chloroform to remove Di-MeAm before using Ethanol to remove further Amm. Cl. Why not do it the other way around ? ie purify with Ethanol 1st, then wash with Chloroform. Seems like this might use a little less Chloroform, which is more expensive and takes more work to obtain than the Ethanol. LaBTop (Moderator) 02-01-00 10:40 No 123294 Same answer as 5 posts above. Rule of thumb is allways removing the impurities first, then you don't have to worry about their influence on the rest of the procedure. And it looks as if you'r the trial and error type, please, do first the proposed method, report back here, and THEN start experimenting with own ideas. This mixing up of good recipees with own ideas at forehand (without telling it), has caused a lot of misunderstanding on this board, you have to pull the truth out ,before you can see the obvious wrongdoing. This gave a lot of good advice/recipees a bad "press" at the start of experimenting by other members.(most of them with minimal chemistry background; strange thing is, however, they seem to have the best enthousiasm level).  LT/ Ultraman (Member) 02-01-00 10:47 No 123295 Point taken. Thanks for all the input guys. Will report back - hopefully with  results. Starlite (Member) 02-01-00 13:28 No 123296 LaBTop: What's the date on your Vogel...I have a '57 and a '62 but they only give the acetamide process...pg # pleeezzeee, I may have to get another one! thx! LaBTop (Moderator) 02-01-00 15:11 No 123297 First published 1948, Code Number: 85288. The Preface by Arthur I. Vogel is dated December 1946. LT/ Ultraman (Member) 02-01-00 22:32 No 123298 Where can the older editions be bought ? LaBTop (Moderator) 02-02-00 03:39 No 123299 If you'r lucky, in a specialized second hand bookshop. You can't order them allready for a loooooong time anymore. And you have to thoroughly search the shelves yourself in the chemistry or physics corner. You will find many more hidden treasures there. LT/ Ultraman (Member) 02-04-00 12:49 No 123300 Godzilla thought about the Bright Star Procedure for MeAm and this is what he suggested: 1. Followed BS instructions exactly. (Used Lab grade Paraformaldehyde, Lab grade AmCl) 2. Heat slowly - took one hour to reach 104. (Consider this Time=0.0 Hours) 3. Held at 104 for 5.5 hours. Used boiling stones and stirbar on slow. 4. At T=5.5 hours turned up heat. Attempted to vary stirbar speed to induce distallation and keep temperature at 110 or less. Note: 1st 125 ml came over while mother liquor was at 110 C. Next 75 ml came over at about 115 C. Last 25 ml came over between 115C-120C. (all temps are mother liquor) 5. At T=9.3 hours distillation got painfully slow, and was nervous about 120 C temp. There was approx 275 ml of stuff in recv flask. Took boiling flask off heat, poured into beaker and placed beaker in ice bath. Mother liquor was a very light golden yellow with a faint odor of fish. Sometimes it almost smelt like Oreo cookies, but that might just be the other shit trying to cover up all the funky smells. 6. In about 5 minutes AmCl crystals began to form. Started getting nervous that the whole beaker was going to become AmCl crystals and nothing else. It became very full of AmCl. 7. Poured beaker contents into vac buchner funnel and obtained approx. 250ml of very light golden yellow filtrate. Recovered 25.9 g of slightly moist AmCl. 8.At T=9.6 mother liquor was back at distil. Mother liquor temp was at 118 C, oil temp was at 137 C as distillate came over. 9. At T=11.0 125 ml had distilled. Mother liquor temp was now at 125 C. Turned on Vacuum. 10. Vacuumed away until no more distillation occured. 11. Product weighed 104.9 g before purification with SLX denatured Alcohol. Was a white-very light yellow mixture just a described by Bright Star. Very soggy, a small stick will stand up straight in it. 12. Poured boiling SLX into product, stirred vigoursly and vac. buchner filtered. 13. Recovered an additional 25.9 g of AmCl. (This AmCl smells slightly of fish and passes the 20ml/5g NaOH test, but I figure it is too pristine white to be MeAm. It is also more hygroscopic than the AmCl from the previous AmCl filtration. 14. Boiled away SLX/product until boiling ceased. Mixture was same color, but syrupy. 15. Poured mix into container and put in freezer. 16. After a while - checked mixture. It was a very frozen slush. Came out of container in one chunk. 17 Now have 99.4g of very wet, yellowish white product. It still looks like it is frozen, but is at room temp. The color reminds one of a yellow snow cone that someone has sucked all the flavor from. 18. Don't know what to do with it now, as no dessicator or centrifuge available. How the hell do you make a centrifuge ? LaBTop (Moderator) 02-04-00 09:26 No 123301 Go to a household store and get yourself a vedgetable centrifuge( a plastic wireframe basket within another solid plastic basket, with a lid on it and a handle, connected to a plastic gearbox in the lid.) You hang a peace of linen in the wireframe basket, fill your goodies in it, at the outside of the bottom, close the lid and start milling like a crazy coffeegrinder. Your liquids go through the linen, your goodies are as good as dry. Hang your goodies in the linen in a widemouth glass bottle, with a bottom full of dry NaOH pellets, and close the bottle with a rubber/cork stop, which holds the linen. Eventually place the bottle now in a hot water bath, fix it, that it won't fall over. A much faster method is to crunch your lump of goodies, put them in your destillation flask and set the oil on 75 C and put full vacuum on it, untill totally dry. You will see that at the end, suddenly the mass will turn into dryness. Preferably use a Rotavap for it, but when not in your posession( sell the car, a good cook offers anything for a good "meal"!), use a fixed vacuum set-up. The color indicates you still have contamination in it, probably sodium formate and methylal. You did not really read my Notes. And you still don't understand all the washings and what they do. Combine BS method with the knowledge I gave you, and the next time, please post the URL to BS method, I don't know what is meant. LT/ LaBTop (Moderator) 02-04-00 09:30 No 123302 For a reasonable cheap self to build Rotavap machine, see here: Post No 123387 LT/ Ultraman (Member) 02-04-00 19:59 No 123303 I read that chloroform dissolves di-MeAm. Does it also dissolve sodium formate and methylal, and leave our friend MeAm ? LaBTop (Moderator) 02-05-00 15:05 No 123304 read first this: ""digest the semi solid residue with chloroform ( to remove the dimethylamine hydrochloride), filter off (note 2) the methylamine hydrochloride (about 20 g.) at the pump and wash it with a little chloroform."" What does this teach us? That you can wash MeNH2 with chloroform, so it will not dissolve too well in it, otherwise another solvent would have been chosen. n this: ""Purify the crude methylamine hydrochloride by placing it together with 250 ml. of absolute alcohol in a 500 ml. round-bottomed flask fitted with a reflux condenser carrying a cotton wool (or calcium chloride) guard tube. Heat the mixture to boiling for about half an hour, allow the undissolved material to settle and decant the clear solution. Cool the solution and then pure methylamine hydrochloride will separate : filter (note 2) and use the filtrate for another extraction. Four or five extractions are required to extract all the methylamine hydrochloride."" What does this learn us? That you must do four or five extractions( in this case you could better talk about recrystallisations), with PURE (no water!)alcohol (ethanol or methanol or isopropyl alcohol etc.), to obtain PURE MeNH2. It's a bit of work, but: Proceed please LT/ Ultraman (Member) 02-06-00 03:19 No 123305 You got it BIGTOP !!  I was hoping to squeak out of a little work by not having to reflux. Been there with the MeNH2 on previous attempts. Guess I'm just looking for the easy way out. Was hoping that the boiling SLX would be good enough. Hey. Got the centrifuge today. It is one kick ass son of a bitch. You can either crank it by hand, or when you get tired, you can use your foot. I love it. Can't wait to try it out. Also found an xcellent desicator. A mason jar with a big old rubber seal. What kind of linen do you prefer ? Also, I know this is a stupid question, but I'm gonna ask anyway. How pure does MeNH2 have to be to make honey ? Next time Godzilla and UMan try, we'll post it as a new topic as you suggested. Damn, I'm really start to appreciate the work involved in org. chem labs !! Take care and be good. And thanks for sharing your wealth of knowledge. Over and Out. UMAN. CHEMMAN (Member) 02-06-00 03:35 No 123306 Methylamine was my first ever chemical venture.I followed Vogels synth( library). It works fine Formalin and ammonium chloride. When he says concentrate to half, you need a vacuum source preferably to distill half of the water away. When the vessel cools it will be ammonium chloride that falls out. It Liivess. LaBTop (Moderator) 02-06-00 18:49 No 123307 ""What kind of linen do you prefer ?"" Any fine woven pillow cover or T-shirt will do, Check in the wash-mark that no other sources than linen are used, must be 100%. ""How pure does MeNH2 have to be to make honey ?"" This is a hobby-horse of me: try to get your ingredients as pure as can get, so you don't have to ask here: what the hell went wrong? Or start a thread on a good synth, saying that it don't work.(should add: for me!), because of lazy, slobby precursor purification. I get the chills when somebody proudly announced: and then I proceeded with my beautifull, RED coloured ketone( MDP2P, P2P), and the sucker don't even realises that when it's red, he should purify it first, it should be light YELLOW. How many times do I have to YELL that here........ LT/ LaBTop (Moderator) 02-06-00 18:53 No 123308 And you still did not post the BrightStar URL, so we all know then which syntheses you use, when we discuss it in this thread. LT/ Niels Bohr (Member) 02-06-00 22:01 No 123309 If you are having a problem finding formaldehyde solution, go to the pharmacy and ask the pharmacist for 37% formaldehyde solution. It is sold by the gallon for < $10. I got mine at Rite Aid - no questions asked. Tell them that you are going to perserve fish, frog eggs, or pork rinds for fishing bait. When you use the solution from the bottle, replace the leftover into a smaller bottle where the formaldehyde takes up the entire space in the bottle so as to exclude air, else it will polymerize into paraformaldehyde (white flakes in the solution). Keep at room temperature and do not refrigerate because it will accelerate this polymerization. LaBTop (Moderator) 02-07-00 14:17 No 123310 Easier solution: buy such a opened wine bottle preserver thingy ( a small hand driven vacuum pump with a needle attached), and slam the needle through the rubber stopper you gonna use to close the bottle with formaline. Then pump all air out, and let the wine thingy sit there, or pull it out. And eventually close the minuscule opening with a greased plastic toothpick, only stuck in half deep. Grease the sides of the rubber stopper with vacuum grease, not too much, but all around it. LT/ Ultraman (Member) 02-07-00 20:37 No 123311 Awww hell, sorry LaBTop. Thought you meant next time post as BS sythn on new thread. The synth is at: http://lycaeum.org/~rhodium/chemistry/mdmasyn.txt Ultraman (Member) 02-07-00 20:42 No 123312 CHEMMAN - Are you saying that after the flask is cooled for the 1st time, and AmCl crystal filtered - you put flask back on heat and applied vacuum ? To speed up subsequent distillations and keep temps lower I presume ? What was your yeild ? What was your starting amounts ? Ultraman (Member) 02-07-00 20:59 No 123313 Continuing dream from post 02-04-2000 12:49 AM above: 19. Several Days later yellow mush was placed in coffee filter and allowed to drain overnight. 19.5 Remaining mush in coffee filter was washed with enough Chloroform to cover the mush and make if fairly liquid. 20. This was then brought to vac. buchner where a very sparkly crystilline and white crystals were left on the filter - approx 19 grams. 21. The yellow filtrate was washed again in Chloroform and an additions 1.5 grams were recovered - looked just like the 1st batch. 22. Crystals dissolved in 18 C deg SLX very easily. 23. Crystals passed delequesence test. 24. Crystals brought to centrifuge and then to the "dessicator". Possible mistake - might should have tried recrystallizing stuff that drained from coffee filter. May have lost a little yeild, it was a significant amount of liquid - 25 to 50 ml (didn't measure) QUESTION ABOUT centrifuge : Do ya cover the entire centrifuge in the linen and lay the crystals at the bottom without any further protection to keep them from flying around ? Ultraman (Member) 02-07-00 21:04 No 123314 Thanks for the tip Neils. It just happened that Godzilla had some PARA buried in his backyard so UMAN thought he'd give it a whirl. Hoping to try the liquid stuff next round. ChemHack (Member) 02-08-00 14:13 No 123315 quote: --------------------------------------------------------------------------- "Also, I know this is a stupid question, but I'm gonna ask anyway. How pure does MeNH2 have to be to make honey ?" --------------------------------------------------------------------------- The answer is that it depends on your method of amination. # If you use the Al/Hg method it doesnt have to be very pure at all because it calls for a 300% of the of methylamine that is actually need. (amine:ketone approx 3:1). # If your so called methylamine is 50% ammonium chloride then you are still have a 50% excess of methyamine (3:2 ratio). # The ammonium chloride isn't very reactive with the Al/Hg method so you don't really have to worry about it making MDA before you get your MDMA. # Now if you plan on using the cyno- amination instead of Al/Hg then it WILL matter. ChemHack (Member) 02-08-00 14:15 No 123316 Oh yeah, a lot of that melted stuff prolly had some goodies. Oh well. Niels Bohr (Member) 02-08-00 18:22 No 123317 In case anyone has not figured this out yet, ChemHack is the expert on this subject, so just do a keyword search on methylamine and his name and spend the day reading. Lots of good info - thanks ChemHack WISDOMwillWIN
	LaBTop (Daddy) 02-10-01 00:23 No 172622		Re: Detailed Methods for Non-chemists . edit 6feb1	Bookmark Reply
			DMF O2-Wacker : Safrole to MDP2P. KrZ (Hallucinogenius) 11-07-00 11:31 No 67435 Let's look at the literature (LT/ : editted for readability) : 3.24g PdCl2 32.40g CuCl2.2H2O 324.36g Safrole 70mL H2O 500mL DMF (DiMethylFormamide) Placed everything except the Safrole in a 4L reactor, stirred heavily exposed to atmosphere for 4 hours, till all compounds were dissolved.  Then added Safrole, and removed atmosphere with vacuum. Pressurized to 35 psi O2. Pressure                  Time after drop (psi) Last Drop (minutes) 15 17 15 18 15 20 15 20 15 29 15 38 ~4 30 Total O2 uptake ~94 psi. Repressurized to 35 psi after each drop. Total Reaction Time: 172 Minutes Added 500 mL 5% HCl to reacted solution. Separated precipitated Ketone/Aldehyde. Extracted the 5% HCl solution with 3x 100mL DCM and separated those, and pooled the 3 DCM/ketone extracts with the precipitated Ketone. Clean up : Washed pooled extracts  2x with 300mL Saturated Sodium Bicarbonate solution and separated pooled extracts each time. Washed pooled extracts with 400mL distillated H2O and separated H2O. Washed pooled extracts with 400mL Brine Solution (saturated NaCl) and separated again. Dried extracts with 50g dry Na2SO4 for 45 minutes. Filtered to Remove Na2SO4. Vacuum distilled at ~2.0mm Hg to recover 311.22g PiperonylMethylKetone (MDP2P) fraction between 105-114C.  There was an Isosafrole forerun, and a minimal high boilingpoint and thus polymerysized glop after 114C. Molar % Yield: 81% A confirmation of above procedure by Grouch : Grouch (Old Hiver)02-05-01 10:58 No 171271 I just confirmed that the 35psi O2 DMF wacker works fine.  I used a Nalgene 20L polypropylene carboy and I drilled a hole in the cap and used a threaded long stem tire valve with a nut and washer and rubber grommet.  I also used a 3'' stirbar and a Thermoline heavy duty stirrer that's rated to stir up to 132 litres.  I pressure tested the carboy to 50psi with scalding hot water and stirring for 5 hours and there was a bulge at the bottom but I'm guessing it could even hold much more psi. Edit : Nalgene Carboy Warning!! For those who saw the O2/DMF/CuCl/H2O/PdCl2/safrole thing in the 20L carboy, on the second try, right when the reaction was complete, I noticed after I picked up the carboy, a few ml's leaked out.  There were a lot of little cracks all around the bottom sides of the container so choose a better one. End Edit Here's my data: Inside the carboy I placed the following: 30g PdCl2 165g CuCl (not CuCl2) 669ml water 4600ml DMF I stirred this thing uncapped for close to 3.5 hours then I added 3kg safrole, then capped it and tightened the cap with a BoaConstrictor strap wrench from Canadian Tire, and pressurized it and purged it 3x with O2, and then I took it up to 36psi and started stirring.  I checked the psi every 20 minutes exactly and topped it back up to 36 psi: time        drop in psi 0                 0 20min             10 40min 11    getting warm 60min 7 80min 12    getting hot 100 12.5  hot to the touch, but still touchable 120 12 140 9 160 8 180 5 200 4     still hot After the reaction, I dumped it into my 22L sep funnel which is made from a 22L heavy walled SHOTT RoundBottomFlask, and then dumped in 5L of 5% HCl.  I allowed this to cool for a few hours.  When I returned, I let the crude ketone come out and there was already about 2750ml.  I then extracted with: 3x1L DCM The combined extracts and crude ketone was then washed with : 2x3L saturated sodium bicarbonate (528g/6L) Skipped KrZ's water wash 1x4L saturated sodium chloride solution (1250g NaCl/4L) Then I dried it with 551g sodium sulfate for 54 minutes then evaporated the DCM to get 3124g crude ketone then distilled to afford me with 2500g ketone (76% molar yield!!!)   Grouch (Old Hiver) 02-06-01 01:48 No 171396 The way you shake it is by stoppering it and carefully lifting it out of the 'wooden chair with a 6" hole drilled in it' hacked stand, inverting it and resting the shoulder of it on one knee while taking the stopcock side and shaking/swirling it and venting it.  When finished, carefully put back, unplug and let settle.  The 22L flask was originally just a plain SHOTT RBF but modified by a glassblower with a joint on the neck and a stopcock at the bottom. CuCl instead of CuCl2?  Reason not really important; you can use a little less and have less Cl- ions around.  Solubility may be different in different solvents, but I haven't checked.  I like the colors more using the CuCl left over from over two years ago back in the days of the 'balloon on top of the flask, ton of catalyst' Wacker. Above procedure is pretty much EXACTLY the same as KrZ's post a long time back in a thread called 'o2 is shit' or something like that where people were, for wrong reasons, doubting the procedure.  The ONLY change is the CuCl and the scale and equipment used.  I copied it almost EXACTLY. The reason for the erroneus pressure decrease at 60min was likely due to me not setting the stir speed as fast as the other times.  And NO, I wouldn't have used the word 'confirmed' if the reductive amination failed. PS:  The wooden chair had to have been in your family's home and be a minimum of 43 years old and re-painted a few dozen times by your father, or none, ABSOLUTELY NONE, of the above procedure will work. WISDOMwillWIN
	LaBTop (Daddy) 02-12-01 17:19 No 173000		Re: Detailed Methods for Non-chemists .edit 13feb1	Bookmark Reply
			Detailed Methods for Non-chemists. edit 19feb2001 XII.MDMA via LEUCKART, SMALL TO HUGE SCALE. http://rhodium.lycaeum.org/chemistry/leuckart.txt Huge scale Leuckart MDMA manufacture by LaBTop. http://rhodium.lycaeum.org/chemistry/mdp2p.leuckart.txt MDMA via the Leuckart reaction http://rhodium.lycaeum.org/chemistry/asarone.wacker.txt TMA-2 from Calamus oil: Wacker Oxidation of asarone, followed by Leuckart amination XIII. SAFROLE to MDMA, BRIGHT STAR SYNTHESIS http://rhodium.lycaeum.org/chemistry/mdmasyn.txt Complete MDMA Synthesis by Bright Star XIV. RHODIUM's MULTIPLE PREPARATIONS of ISOSAFROLE The latest findings of Rhodium for preparation of Isosafrole : http://rhodium.lycaeum.org/chemistry/isomerizafrole.html and the preparation of the Alumina/Sodium catalyst for nr 8 : http://rhodium.lycaeum.org/chemistry/uspat3852305.html Pay also attention to : Safrole + 1-Butanol +4M KOH at conventional reflux for 15 minutes gives 99% Isosafrole in nr 4. Nr 7, solventless PTC variation is covered under my Isosafrole writeup in this thread. LT/  WISDOMwillWIN --------------------------------------------------------------------------- --------------------------------------------------------------------------- Here is that info how to make d- or l- isomers of your drugs. Serious Chemistry :  MDMA chirality  All 22 posts ChEss_Piece_Face (Stranger) 07-15-00 00:28 No 28995          It occurred to me that MDMA is chiral, and most chiral pharmaceuticals have only one active isomer. For example, only the S isomer of ibuprofen is active, although the R isomer racemizes over time in the body. Pure S is therefore more potent and faster acting than a racemic mixture, which is what is usually sold OTC. Does anyone know which isomer of MDMA is the active one, and has anyone toyed around with making enantiomerically pure MDMA? I happened to notice the other day that Aldrich sells MDMA.HCl!!! It just so happens that they sell one of the pure isomers in addition to the mixture. gaston (Hive Bee) 07-15-00 03:57 No 29040 The S isomer, as with methamphetamine: http://www.erowid.org/library/books_online/pihkal/pihkal109.shtml JOESTALIN (Stranger) 07-17-00 07:02 No 29651 actually it is the R isomer of Extacy THAT IS THE active isomer as it was proven in a J. Pharm. CHem. article in 1984, and to obtain an optically pure isomer of E is about as expensive and time consuming as the synthesis itself with no increase in yield. john_galt (Stranger) 07-17-00 13:11 No 29757 From what I read in PIHKaL, it is actually necessary for the desired effect of MDMA to consume the racemate. "A penny saved is .72 pennies earned (after capital gains tax)" -John Galt JOESTALIN (Stranger) 07-19-00 05:45 No 30453 When was the last time someone ran into an illegal drug that was racemically pure, huh? Rhodium (Chief Bee) 07-19-00 06:02 No 30464 Last weekend I saw a couple of guys snorting coke. Coke is pure l-cocaine. john_galt (Newbee) 07-19-00 16:01No 30683 Don't be silly, dude, NONE of the popular synths for MDMA are enantioselective. They produce both enatiomers at equal rates, therefore, all of them produce the racemic modification. Resolution would involve recrystallization of a salt with 2 chiral centers of an enantiomerically pure acid(thus producing diastereomers with differing physical properties) or chromatography. -John Galt Rhodium (Chief Bee) 07-19-00 17:33 No 30705 None of the MDMA sytntheses, no, but I don't think anybody said that either. JOESTALIN (Stranger) 07-20-00 10:03 No 30967 what I meant to say was no designer drugs and cocaine by definition isn't really illegal doctors still presribe and use it... i do mean use it john_galt (Newbee) 07-20-00 13:33 No 31015 When someone insinuates that one never encounters a completely racemic drug, he is inevitably implying that there is some sort of enantiomeric excess. With the popular MDMA synths, this is impossible. I was just using basic theory to show that, indeed, *ALL* of the XTC that people consume IS racemic, as that is what the dude was asking. -John Galt ChEss_Piece_Face (Stranger) 07-20-00 20:44 No 31163 No, I wasn't asking if street ecstasy was racemic or not, I'm quite aware that it is. Rhod had it right, I was wondering if any curious bees had tried to isolate the active enantiomer. This could either be done as in J-G's post, or via ring closing, then opening rxns (you can get pseudoephedrine from ephed/pseudoephed racemate this way). I guess no bees have gone there. gaston - thanks for the link with relevant info. I've only been at this for a little while now, so I didn't even know PiHKAL was online! LD_50 (Stranger) 07-21-00 03:54 No 31278 ok...we all seem to agree that the standard synth produces many enantiomers and as such is a racemic mixture. and using a chiral "agent" would be usefull in seperating them into thier 2(?) diastereometric salts. now if we had mdma as a mixture of the s and r forms in (aq.) soln. (R)-(-)-MDMA and (S)-(+)-MDMA....and used (+)-tartaric acid to this soln. this should precipitate out the (S)-(+)-MDMA from solution (by using molar equivelents of the +tartaric acid?equivelent to the amount of the different sterio isomers?).....then follow with (-)tartaric acid for the (R)-(+)MDMA but,like in methamphetamine, this could compose as much as 50% of the total product...so we perhaps have a slight problem, for wasting half of the product for recemic purity is very unfortunate indeed... So the problem seems to be converting the (S)MDMA to the prefered (R)MDMA after seperating the racemic mixture?????? now temperature during the synth to mdma is probably a big factor in determining if r or s isomers are produced and i have heard of using chiral catalists to get racemicaly pure products...anyone know if keeping the reactants in the Hg/Al amalgam process at a low temp might favor the (S) or (R) entomers? Osmium (Moderator) 07-21-00 03:55 No 31279 There are stereo-specific syntheses which produce only the desired isomer. LD_50 (Stranger) 07-21-00 04:17 No 31286 maybe not pre reaction--->(X)MDMA but maybe some kind of catalitic treatment to the (S) isomer after seperating them? But this is not pharmacy 300...and it seems that the (S) isomer is active and not unpleasant...but is definatly less prefered than the (R) isomer....now if it was temperature dependant on what isomer was producduced in greatest quantity then tight controll of the reaction could produce fairly easy controll. I am wondering if having the reaction proceed at a low temperature(in coolant,methylene glycol etc<antifreez>, and a refrigerator coil @ 0 degrees centigrade might be better<but maybe very slow> it would be really nice to have a spectrophotometer at home. phree_radikal (Stranger / Eraser) 09-29-00 18:23 No 55828 Firstly, there seems to be a descrepency between published articles on whether it's exclusively R or S... sources I read implied the S was active and the R not. The significance of this, as I see it, is that 50% of the propanone is effectively sacrificed at the step of reductive amination. I'm not quite down with the mechanism yet but that's gotta be when chirality is introduced... if you know the mechanism (which some of you do, I'm sure), then you can predict the product distribution or whether it's entirely racemic (equal distribution). What I wanna know is whether any one has a stereoselective synth for the active enantiomer? Please, please, pretty please? FarQ (Hive Bee) 09-29-00 22:32 No 55890 In my understanding of Shulgin's writings, is that while neither isomer is inactive, one produced more effect. Neither effect was as good as the synergictic effect of both together. So WTF you wanna seperate them or worry about stereo specific synthesese? phree_radikal (Stranger / Eraser) 10-02-00 20:24 No 56743 So we can verify the research of others... If it's true they're synergistic, then I'm not going to do more work for reduced effect. That's silly. But I am curious about which is which and what the difference in effect is. I gotta feel it. p_r LaBTop (Daddy) 10-11-00 11:06 No 59321 Here is some more in-depth info on the subject : Ref.: 'Quasar' Research Monograph 22. Absolute Configuration and Psychotomimetic Activity. G.M.Anderson III, Gisela Braun, Ulrich Braun, David E. Nichols, and Alexander T. Shulgin. This paper is 8 pages long, so I will highlight the most relevant pieces of it, relevant to the questions and answers (which are all not precise enough or even erronomous to fully understand the matter). Exerpts: Most of the known psychotomimetic agents have at least one chiral center within their structures but have been studied only as the racemic mixtures. All of those which have been studied in optically  active form are consistent in that the more potent isomer is the isomer with the absolute "R" configuration at the chiral center carrying the nitrogen that correspondents to the amino group of the phenethylamine moiety. (Follows a long list of isomers and their potency in humans). Finally, the "R" (levo-rotatory) isomer of 3,4-methylenedioxyphenylisopropylamine (MDA) is reported to be three-fold more potent than its optical enantiomer (Marquardt 1978). With MDMA this potency assignment is reversed ! "S"-MDMA is more effective as a CNS agent than is "R"-MDMA. Amphetamine (a stimulant, not a psychotomimetic drug), on the other hand, has the "S" or dextro-rotatory form that is the more axtive. (+/- twice as more potent as the "R" isomer, Smith and Davis 1977). The 3 chemical species : racemic MDMA, "R"-MDMA and "S"-MDMA, were evaluated in normal human subjects as their hydrochloric salts, orally. Judged as -, +\-, +, ++, and +++. The data represented 35 clinical trials. (follows a plotted graph with 3 lines through data points. The "S"-line is the highest, a +++ at 120 mg dose, followed by the "dl"-line,racemic, a +++ at 160 mg, and the "R"-line with only one + at 200 mg). It is concluded that the "R"-isomer only slightly interveres the effect in the racemic sample, compared to a pure "S" sample, in contrary to nearly all other psychotomimetic drugs. Qualitatively, most of the sensory and interpretative properties reported for the racemate are seen in the "S" isomer, including the frequent physical toxocity manifestations of mydriasis and jaw-clenching. The "R"-isomer is free of both side effects, even at the highest doses assayed. It must be concluded that (in contrast with the previous generality that the activity of racemic psychotomimetic compounds could be largely accounted for by their "R" isomers), with MDMA, the active optical isomer is the absolute "S"-isomer, with the configuration of dextro-amphetamine, so d-MDMA. ** As an answer to the last question, one direct synthesis for the preparation of the two freebases "R"(-)MDMA and "S"(+)MDMA (with "R"-MDA as another possibility as an extra) is as follows : MDP2P is coupled with "R"(-)benzylmethylamine [ "R"(-)CHNH2CH3 ], and the resulting Schiff base reduced with Raney Nickel. Catalytic reduction of this "R,R" secondary base provides "R"-MDA (nice aint it, precisely the right, most active MDA isomer, keep that in mind!), (alpha)D= -24.7, agreeing with literature and bought sample from reliable source. This base is formylated in methyl formate in a sealed tube, and the resulting formamide has a reversed rotation (alpha)D= +12.4 (in ethanol) and a m.p.=99-101. Reduction of this amide in THF with LAH provides the desired "R"-MDMA, (alpha)D= -18.2, m.p.=181-183 as the HCl salt. The "S"-isomer can be prepared in an exactly parallel manner (with "S"(+)CHNH2CH3 of course), with the primary amine showing (alpha)D= +25.3, the amide (alpha)D= -12.6, m.p.=101-102, and the final "S"-MDMA with (alpha)D= +17.2 and a m.p.=184-185. Racemic MDMA m.p.=150-151. "R" = levo "S" = dextro dl  = dextro/levo (racemic mix) May I conclude for you all, the synthesis of specific isomers for MDMA is useless. The difference in effects felt for the "S" isomer and the racemic mix are neglectible ! The synthesis of the d-methamphetamine isomer however, compared to the racemic mix, dl-methamphetamine, is surely worth the trouble, it's effects are noticably different, especially the fucked up state connected with orally administering the dl racemic mix is smoothed down exessively. The synthesis of "R"-MDA is also worth the trouble, find out yourself if you'r the investigating kind of person. The synthesis of a racemic mix of dl-methamphetamine into the pure d-form has been posted by Spitball/Drone: http://hive.lycaeum.org/ubb_board/Forum6/HTML/001137.html  Let's Go for the gold.. 05-27-99 11:00 AM : 15 g d-tartaric acid and 12 g dl-methamphetamine.HCl 300 ml Ethanol >98%. Heat the ethanol to a boil. Slowly, add both d-tartaric acid (a whitish powder) and dl-methamphetamine till both totally dissolve, surplus heat needed when too slow, until boiling again. Then put the closed flask in the freezer and see the crystal needles formed after a few hours.  That's d-methamphetaminebitartrate acid crystals. Filter the crystals off. An acid/base extraction and then gassing of the freebase with HCl gas gives d-methamphetamine.** LT/ : NO ! This procedure gives you the unwanted  l-methamphetamine !!! And dwarfer gave us 2 patents explaining the matter a bit more elusive: British patent nr. 508757 US patent nr. 2276508 Also look at the VillageIdiot pages: http://www.angelfire.com/de/VillageIdiot/isomers.html http://www.angelfire.com/de/VillageIdiot/racemateresolution.txt Now, after reading the US patent, I must say, I've never seen a more unreccognisable form of english explanation before. I understand that the above method is not the same as the one outlined in the British and US patent, indicating that with above method from Spittbal, you get l-methamphetamine. TO DO IT RIGHT : The British patent however is as follows, in simple understandable text: 85 Parts of racemic methamphetamine are introduced into a solution of 100 parts of d-tartaric acid in 1000 parts of methyl alcohol. After protracted(what's that?) standing, about 100 parts of the precipitated salt are aspirated off and extracted with hot ethyl alcohol. Since the d-tartrate of dextro-rotary methamphetamine is readily soluble in both methyl and ethyl alcohol, whereas the d-tartrate of levo-rotary methamphetamine is sparingly soluble both in methyl alcohol and hot ethyl alcohol, an extremely simple separation of the d-tartrates of the optical antipodes of the base is effected.** In my opinion that means that you must filter off the unwanted l-methamphetamine-d-tartrate crystals precipitated out of the solution, (better recrystalize a few times more by evaporating more solvent and cooling again, to obtain a pure solution of the d-form!) and add a strong base (KOH, NaOH) to the remaining solution until pH 13 to force the freebase d-methamphetamine-d-tartrate out as an oil. Then separate the oil from the solvents, and distillate to be sure, and then gas that clean oil with HCl gas to exactly pH 7 to get your d-methamphetamine.HCl salt. Filter and dry. I hope this error has not given too much of trouble to experimentors in the past. They made then the wrong l-methamphetamine following those instructions. Correct me if I'm wrong. LT/ --------------------------------------------------------------------------- WISDOMwillWIN    buchiguy (Stranger) 10-12-00 14:03 No 59546 Cheers to Labtop! Thanks for clarifying that for my imaginary friends as they were ready to abandon the sodium borohydride reduction, speculating too much of the racemate being produced was weakening the product. If memory serves me correctly, you were partly responsible for that great post on the borohydride reduction to begin with. Definately one of the easiest reductions my imaginary friends have seen and the yields are great! Any suggestions for getting away from methylamine gas though? Stinks up the neighbourhood. My friends built a nice scrubber but doesn't completely do the job. LaBTop (Daddy) 10-24-00 03:43 No 62904 "R"(-)benzylmethylamine [ "R"(-)CHNH2CH3 ], and "S"(+)CHNH2CH3 : can anybody close to chemical suppliers provide us with the prices of these chems, and tell us if you can order them at all ? Did you really all miss the importance of this easy route to the most potent isomers of MDA and MDMA in pure form? Expected some more reactions. If these 2 isomers of benzylmethylamine are obtainable of course, or could be -easily- created in your garage ! The sources I have access to have no info on these compounds. Psychokitty, do you have access ? Anybody ? The rest of the steps is childsplay. LT/ --------------------------------------------------------------------------- WISDOMwillWIN LaBTop (Daddy) 10-24-00 05:07 No 62922 Missed that last question from Buchiguy : If you follow all the OnePot directions shattered over the board, and use some McGuiver techniques, you will virtually smell nothing. Use a exhaust fan connected to a box with a in and out opening, with clothhangers in it, 5 to 10, and hang well wetted towels on them, alternating 5 cm above the bottom and the next one touching the bottom, so you create a labyrinth where the air is forced to follow a S-shaped route to the end of the box. The water in the towels will absorb all traces of MeAm gas escaping your setup, especially during the adding of the boro. The clean air will be exhausted out of your working space. Wash the towels periodically in lots of water and use rubber gloves for that. You pump (gearpump in case of 100th of liters) your 10% MeAM/MeOH mix into your vessel, or syphon it in, this will also prevent any gas from escaping. All open pipes must have washing bottles attached. Adding boro in one with a funnel means you must have another pipe with a big ass washing bottle attached, filled with 10% HCL/water solution, to effectively kill all MeAm smells pushed out by the pressure, building up, when adding boro. And have another EMPTY washbottle in line before that one, to trap suckbacks, or you have WATER sucked in the reactionvessel when you loose pressure suddenly ! The rest of all your entrances to the vessel must be airtight !!! While adding boro, you have the exhaust fan intake hose placed near to the funnel, so it takes away directly all fumes escaping there. Stopper the funnel loosely inbetween addings, or the stopper will pop out, caused by the pressure buildup. Especially airtighten your big lid, which you use to climb in and clean the kettle afterwards, or the other use of this opening for taking out the 100 kg powder produced in the same kettle with a  big ass coal shuffle from SSteel(your 90 liter clean base with the 270 liter acetone, and then bubble HCl gas through, while mixing). First shuffle the powder away from the valve tap opening in the center of the bottom, or that will be stucked with powder at the end. Then you open that valve for 2 seconds to clear the valve, close it again, remove the first bucket with some powder and acetone in it, and then open the valve a bit again to let the clear acetone slowly out, not disturbing the pile of powder inside the vessel, into several buckets, until no more acetone comes out, close the valve and start gold digging with your shuffle ! Have fun ! The last rests of powder you wash out with the acetone you decant off from the buckets where you shuffled the wet powder in (remember, the result of the crystallization is a big wet mass of toothpaste-like powder mass), and wash the powder, left in the kettle, out into the new bucket you placed under the big ball-valve in the bottom center. At the end of the 36 hrs reaction,  after adding the 8 x volume of water and tapping your raw freebase, you add a lot of 20% NaOH or KOH solution to your lots of waste water, till pH 13, and then a lot of 33% HCl solution again till pH 7 or slightly lower. This will break up all hydrocarbons. You now have a non-MA smelling solution, it will have a slight perfume smell. It's neutral, it will not be destructive to plant and animal life. LT/ --------------------------------------------------------------------------- WISDOMwillWIN Acme (Hive Bee) 11-02-00 19:56 No 66110 Acme's route to "R"(-)benzylmethylamine : [ "R"(-)CHNH2CH3 ], Starting with D-N-Boc-phenylalanine-OH. React this with Ethylchloroformate, TEA (0 C, 5 min in THF), and diazomethane (as a 0.3M soln in ether), stir 20 min to get the diazoketone. Yield 100% easy chromatography (follow the yellow band). Homologate this with AgClO4/THF/water(few drops) yield 100% (after adding some brine(sat.NaCl) to precipitate silver, filter over celite) chromatography 10% MeOH/DCM or EtOAC/Hex 0.5 OH. Decarboxylate with NaOH, then TFA/DCM to remove the Boc. Voila!  "R"(-)benzylmethylamine [ "R"(-)CHNH2CH3 ]. Use the naturally occurring (cheaper) L-N-Boc-phe-OH similarly to get the S form. WISDOMwillWIN
	LaBTop (Daddy) 02-17-01 23:39 No 174043		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			Feb19 2001 : THERE WILL BE NO MORE ADDITIONS BY ME TO THIS THREAD (or it get's too big and overloads the server access time) THE UPCOMING INFO WILL BE PLACED IN A NEW THREAD ! That space is reserved for : 1. Alcoholic O2 Wackers (Successfull testruns in process). An easy and fast OTC, small to big scale synthesis of MDP2P and friends. Based on KrZ's many inputs. 2. DMSO O2 Wacker (Testruns in process). Idem. 3. All Hydrogenation methods spelled out by KrZ, if we can get his cooperation to explain those methods to me, or to someone who can PM me again, so I can edit them for him in a readable fashion for less gifted members. (PM me?) 4. The rest of his non-Hydrogenation posts, idem. 5. Baalchemists improvements on Methyl_MAn's Nitromethane method. 6. CURBSHOT's nanoscale Meth method. 7. Aquagirls nanoscale Meth method. 8. Dwarfers ideas, sometimes too mystic to get a grip on, for me alone. 9. Ozbee's Sodium metal ether Birch. 10. PtO2 (also called PtOIV), Adams catalyst Hydrogenation by me and that dutch sculptor, for MDMA and MDEA. 11. A real life? working Safrole + H2SO4 route. I doubt it. See TS I+II. 12. Some of Uncle Fester's really working methods, yes,they do, most of them. Will need some input and improvements of our members. 13. Some links to the most valuable info on Worlock's, WizardX's, ChemGuy's, VillageIdiot's websites. 14. Some of Bankrobbers successfull testruns. 15. List of links to Rhodiums page's most easy procedures for beginning chemists and cooks. 16. Ymirs long forgotten excarvations of old text books. 17. A long list of Psychokitty's references to feasable methods, f.e. the Sodiumtriacetoxyborohydride and Titaniumisopropoxide reactions, and much more, he has lots of them. Let's combine them with a similar list from RefDrone and LaBRat! (Where are you guys, PM me ?) 18. Photo's, brochures, text from Hydrogenators and the appropriate technique's invalved. 19. An extensive 40 page long description how to make tablets, and all possible fillings, a pharmacological approach. 20. Lots of info on Evaporators, many unknown models to the Hive. 21. Mescaline analogs. 22. Testreports on d- and l- isomeric procedures. 23. Photo's and text of pillpresses. 24. How to make improvised equipment for small and huge scale methods, with photo's. and 25. In another NEW thread, all REAL important computer based knowledge for SAFE and FAST browsing of the Hive and the Web. And ANY other posts or threads or links or own NEW methods/procedures/inventions I forgot, which ANY of you feel they belong in here, and which you can send me by PM (Personal Message) or e-Mail. Don't be shy, I appreciate ANY INPUT!
	LaBTop (Daddy) 09-05-01 03:20 No 210291		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			This is the latest buffered Performic write-up by me, use these guidelines, and it won't hurt to compare them to the earlier one somewhere there above. To help everybody out in this somewhat chaotic 2 year long discussion on one of the most interesting subjects for most of the readers, I offer you the following effusion : A correct timeline of the-Hive's development of the following high yielding procedure is as follows: Ritter first posted on the young Hive, end of '98 a short, buffered Performic acid oxidation, and he used Na2CO3, Sodiumcarbonate as the buffer, and DCM as the solvent, then Beagle posted a similar procedure, and LaBTop posted a short one using NaHCO3, sodiumbicarbonate (a.k.a. baking soda or sodiumhydrogencarbonate) and DCE, where he mentioned that DCM could be used in practice with similar yield. Then Gyrogearloose reproduced that one in practice also, on medium scale, 500 g MDP2P, then LaBTop wrote in april 2000 a very extensive writeup from past practice in the sticky threads, where he advised to use a new find from Osmium to produce the precursing Isosafrole with Aliquat phase transfer catalyst in 5 minutes after the heating reached the boiling point of safrole. Then Baalchemist got enthousiastic and reproduced in practice LaBTops extensive practical MDP2P write-up, and made a few small alterations during the following year. Ritter as the last one posted again, from practice, saying there is no real difference between the use of sodiumbicarbonate and sodiumcarbonate as the buffer salt, and proved it with hard facts, so feel free to use either of these salts. Now Rhodium included this procedure in short form in his latest write-up at his page. LaBTop build all the latest info into his latest extensive write-up, with some important new additions for large scale production of MDP2P, which is mainly different compared to small or medium scale in producing performic acid portions only 1 hour before needed during the proces of adding it to the isosafrole/DCM, thus providing a constant supply of FRESH performic acid, no use of cooling when dripping the performic, and preheating the intermediate  and the 15% H2SO4  before adding them together, which seems rather unimportant, but will increase yield substantially, if also a good professional vacuum source is used, yield percentages between 80 and 90% can be reached! Thanks go to Baalchemist for the last two. And now LaBTop provides you with the latest extensive write-up, because he knows that 90% of the members will manage to majestically misunderstand these ultrashort writeups, because of the nature of this board, 90% non chemists and 10% chemists. * * * * * * * * * * * * * * * * * * * * * * * * * For small, medium and large scale MDP2P ketone entrepeneurs, I would strongly advise to pay full attention to the following write-up. See first Post No 23325, and Post No 184407 to get a grip on the Hive's historic development leading to the following newest procedures to produce MDP2P ketone. After that I advise instead of the messy and time consuming Aliquat procedure mentioned there, to follow the most simple, next procedure, to convert your safrole, vacuum distilled from minimal 85% Asian or Brazilian sassafras oil, to vacuum distilled Isosafrole, and then the LT buffered Performic acid oxidation procedure to produce MDP2P from it : Here's first the conversion from Safrole to Isosafrole done by LaBTop, Osmiums simple route was followed, yields are ~95% without vacuum, ~99% with vacuum : No vacuum: Weight 130 kg distilled safrole and add 2% = 2.6 kg KOH grinded flakes or pellets >98%. KOH flakes are in some countries 85%, the 15% rest is water, check it on the label. Then heat up. At 100 C the eventual 15% water will start evaporating, or, when 98% KOH was used, only a small amount of water will come off. This removal of water is critical to the reaction, water present when refluxing will totally stop all isomerization. Add more heat until all water is evaporated. Then at last connect a reflux condenser vertical on your vessel and continue heating until the safrole starts boiling, without vacuum, reflux will be constant at circa 232 C until boiling stops, that means it has nearly all converted to higher boiling Iso. Do NOT crank up the heat then, but disconnect heating and let cool to roomtemperature. Reaction takes roughly 3 hours for non vacuum. You now have ~95% Isosafrole which you use for the MDP2P conversion step. You could distillate it now, to get >99% Isosafrole, but that seems to be no option for the ones who choose for this approach, they probably have no vacuum source, and ~5% safrole will not really interfere with the MDP2P step. Under vacuum : Same as above, only boil off eventual water first with a normal condenser attached, so you can check for any water present, when eventual water stops condensing in the condenser, change horizontal condenser to a vertical reflux condenser, and keep heating (far under 200 C, boiling temperature depends on vacuum source.) Vac reflux should be done overnight because of lower temp, reactions at lower temps take longer. Start a vacuum reaction f.e. at 21:00 hr and next morning its done, all boiling has stopped and safrole is nearly quantitatively converted to isosafrole. Then just distillate the now isosafrole out of reaction flask, dont distill it completely dry though, because you can add a next batch safrole to that little bit leftover {isosafrole/safrole + all the used KOH} again for a next run. Just add at the next run 50 gram of new KOH to refresh a little. Trying to wash reaction in a sep funnel for purifying is terrible: results in a terrible emulsion that's nearly impossible to break up and ends up in alot of LONG labor and endproduct loss. Distilling is a must for best result. Don't worry about leftover safrole with O's Isosafrole vacuum route, usually all converts. However, if a small amount leftover safrole is present, f.e. because you have no vacuum, it wont screw up the performic route. Notes: No CaO at all, 98-99% KOH only. Make sure the KOH are roughly grind-up solids, (not a liquid mix with water), where you sieved all powdered KOH out for an easier workup at the end, use a nylon insect-screen. Add 1-2% of safrole weight KOH flakes and away you go. Make sure that there is no H2O present anymore when you start the actual reflux!. At atmospheric it runs quicker because of higher temp, ~3 hours. Bring it to a reflux and hold it till refluxing stops. Then you know it has converted to the isosafrole which has a higher boiling point. Vac reflux is much longer, but if you're into yield maximalization, then thats the way you want to go. ~98-99% yield. * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * Here's first Baalchemist's write-up for LaBTops modified performic as he posted it lately, then the second part is scaled to what LT/ would do. This can be scaled up or down according to your wishes, may they always come true : Baalchemist: There is no need to pre-stir for more than 5-10 mins. In a nutshell; With stirring in 2L flask add in this order> 250g Iso, 76.9g Baking soda, 770ml DCM, let stir 5-10 mins. Begin dripping in performic solution (232.2g 35% H2O2, 384.5g 86% Formic acid) over a period of a couple hours. It should reflux slightly during addition,but not a hard reflux.Solution will turn from yellow to orange,keep stirring 24 hours,no less. Allow to sit and remove DCM layer,and extract top layer with a small amt. DCM. Evap DCM extracts, add orange syrup to 2768g 15% H2SO4 (preheated to 80c). Stir for 2 hours, no more. Let cool, 2 layers will form. Remove bottom layer, and extract top layer with some DCM, add this to bottom layer. Evap off DCM and proceed to vac distill ketone. Yield 190g+ Ketone ~76% w/w.     ============================ LaBTop's ultimate procedure : ( If you prefer a small scale procedure, just change ALL kg in grams, and liters in milliliters !! ) PERFORMIC ISOSAFROLE GLYCOLIZATION STEP: In a 1600 liter vessel ( f.e. a second hand stainless steel milktank ), add, in this order (while heavy stirring anti-clockwise, (a must-have is a stirringmotor which can turn clock- and anti-clock wise (^1), otherwise too much oxigen and other gasses from the air will be mixed in; you will notice no vortex, but a 1 cm high and quite wide bubble on top instead) : first:  125    kg Isosafrole, distilled. then:    38.45 kg Baking Soda, NaHCO3, SodiumHydrogenCarbonate 98%. then:   385    liter DCM, CH2Cl2, DichloroMethane a.k.a. MethyleneChloride, 98%. Totals to 681.28 kg (weight of 1 liter DCM is NOT 1 kg!). The purpose of the baking soda is to buffer the pH of the reaction in such a way that it doesn't become too acidic, in which case the intermediate monoformyl glycol may undergo oxidative cleavage (and thus lessen the yield). Running the reaction at a higher pH than usual makes more of the epoxide (and thus risk of tar forming) and less of the actual glycol and will decrease yield quite notible. (both will of course form the ketone with 15% H2SO4). Attach a reflux condenser & addition-funnel/container with a dripping valve to the 1600 L vessel. All other openings must be frantically closed with proper tape, or teflon seals, or the reflux will not work accordingly. Leaks will make bad smells. Allow this to stir fast anti-clockwise while you prepare the first 25 liter portion of the total amount of performic mixture : 192.5 kg 86% Formic acid (preferably made by diluting 99% Formic acid) 118 kg 35% H2O2 (hydrogen peroxide), as FRESH as possible, don't use month's old stock. This makes a total of 310.5 liter performic mixture. To prevent such a big amount of performic mixture to get exothermic and too hot, while waiting all these many, many hours necessairy for dripping all of it in the Iso/BakingSoda/DCM mix : Before adding parts of it to the 25 liter dripping container+drip-valve, only 25 (or even 10) liter portions are prepared each time with strong mixing while adding the two ingredients together, and kept in a freezer at around zero degrees Celsius, until needed. Don't cool too deep, it will slow the reaction rate when added to the dripping container and dripped in the vessel. It means that you make during ~half a day, under strong stirring, twelve 25 liter portions and one 10.5 liter portion performic mix, one portion each time, when the dripping container is 4/5 empty. Or even better thirty 10 liter portions and one 10.5 liter portion. That way your performic mix is of a constant FRESH nature, which increases end-yield. The performic acid portions should be prepared in advance (one hour, at room temp: the last 1/5 of the dripping container takes around 15 minutes to empty) to make sure the formic acid has reacted with the hydrogen peroxide (but don't let it stand overnight, or decomposition will occur). Using DCM as the solvent is advantageous, as the reaction temperature can never exceed 40°C (bp of DCM), and by keeping the reaction temperature that low minimizes side reactions. When the 25 liter dripping container is 4/5 empty, refill it from a 25 or 10 liter portion from the freezer. (If your Formic acid isnt 86%, then down to 77% will work, compensate with more H2O2, based on % of formic acid available.) The Formic acid is only acting as a solvent in this reaction, it does not react. Remember, the less performic in the dripping container, the slower the dripping goes, so adjust accordingly, watch the reflux rate AND the temperature, when one of these go too fast or high, close the drip-valve a little, until both reflux and temp are stable again. The technically gifted can make a pressure-equalized dripping container. Slowly, add the performic-mix drop/or smallstream-wise over a 6 to 12 hour period under constant fast mixer speeds. If you add it too fast, the reaction will boil over, and contaminate everything. Use a glass or SS pipe with wide internal diameter, attached to the drip-valve, properly sealed where it enters the top of the 1600 liter vessel, extended just under the fluidlevel, to drip the performic-mix directly into the mass of the fluid, and so prevent too much oxigen or other gasses to interfere with the reaction. It will start to reflux a little, adjust addition rate so it doesnt reflux too hard. Once all performic is added, it will have turned from a yellow to an orangejuice color. Keep strongly stirring for 24 hrs total, no more, no less. (included dripping time). If you stir longer, sidereactions will kick in, lowering the end yield. Note: Remember, do NOT cool the whole reaction mix at all, let the reaction temperature be controlled by the dripping rate! A good double check is the reflux rate, at no times, uncondensed vapours should leave the top of the reflux column! A bad smell indicates this. End note. Turn off the stirrer after these 24 hours, allow the two layers to settle. Separate off the bottom layer (DCM), and extract the remaining top residue-layer 2 times with a small amount of DCM, and add these to the already separated main DCM body. Take this combined portion to a 22 liter Rotavap or conventional distillation machine, distill off the DCM in 15 liter portions, and collect all the resulting orange syrup portions in a heating vessel and heat it up carefully, meaning don't overheat it, to 80 Celsius. All eventual residual DCM, (if any), will evap off (about 5-minutes). You will be left with 183 kg monoformyl glycol, nearly quantitative, 100% yield. Remove the residual fluids from the above procedure for eventual recovery of solvents and clean the 1600 liter vessel with hot, slightly soapy water and then cold water. SULFURIC ACID HYDROLISIS STEP: After the vessel cleaning, pre-heat (^2) the 1600 liter vessel filled with 1384 kg 15% H2SO4 to 80 degrees Celsius. NOTE: Dilute 209.7 kg 99% H2SO4 with 1174.3 kg=liter distilled water for this amount of 15 % H2SO4. Calculation of this amount: 15% / 99% = 0.1515% x 1384 kg total = 209.7 kg 99% H2SO4. 1384 kg 15% H2SO4 - 209.7 kg (99% H2SO4 + 1% water etc) = 1174.3 kg(=also liter) water. 209.7 kg (99% H2SO4 + 1% water etc) x 0.99= 207,6 kg 100% pure H2SO4/13.84= 15.00 % , always double check calculations. NO liters used in calculation here! End NOTE Then add all of the 80 Celsius preheated, distilled orange syrupy monoformyl glycol to the 80 Celsius hot 15 % H2SO4 portion in the 1600 liter vessel. Connect a reflux-condenser on top of the 1600 liter vessel, and be sure there are no other open pipes or joints. Keep the mixture between 75-80 Celsius for 2 hours, NO longer, or again sidereactions will kick in. DISTILLATION STEP: Switch off the heat, and allow to cool back to room temperature. Flooding the reaction mix with some extra H2O prior to extraction helps improve yield because it facilitates separation and fastens cooling down. It will seperate into 2 layers, the bottomlayer is raw MDP2P ketone, which you tap off through the bottom ballvalve. Extract remaining top watery layer with small amounts of DCM (2x, a few liters), tap them off, then add all these DCM portions to already tapped off raw ketone bottom layer. When your last tapped DCM has the same color as when you poured it in, there is no more raw ketone to extract. Then wash and separate this raw ketone 2x with sufficient 5% Sodiumbicarbonate/H2O mixture (a few to 10 liters at a time), to neutralize all residual acid. Check pH first with pH paper, then start adding bicarb until pH stays constant, or even goes up, when adding a bit 5% NaHCO3 again. Then all acid is neutralized. Now place 15 liter portions in a 22 liter Rotavap or newest distillation machine, and vacuum distill the MDP2P ketone  which comes over between 155 and 165 Celsius and lower with the newest vacuumpump, it will begin to come over at circa 20 mBar vacuum and end at circa 1 mbar. A golden, honey coloured ketone will be obtained. Clean the leftover tarry residue in your destillation flasks with acetone, a bit warm acetone will work faster. Yield 76 % w/w, with a Rotavap, about 95 kg clean and pure MDP2P, ready for prefered method of amination. Yield 85-90% with special distillation techniques, about 106.5 to 112.5 kg pure MDP2P. Clean the leftover tarry residue in your destillation flasks with acetone, a bit warm acetone will work faster. AND I DO NOT TELL THE OPPONENTS HERE WHAT THAT TECHNIQUE IS, and will be strongly pissed off when someone else does it openly here, we made their oppressive life already too easy. We have PM's for that. And don't start PM'ing me to ask, only the few I trust to be able to do this can do that, the rest gets no answer. Yes, I'm a prick! ****************************************************************** NOTES: ^1: Easy to construct with a stirrer shaft with a pulley on top, and the shaft leading through two ballbearings, one on top of the vessel, with an extra seal under it to seal the vessel airtight, and one at the bottom of the vessel, to keep the shaft+stirrer rigid. The motor has a pulley attached also, and the belt can then be attached to both pulleys normally, to stir clockwise, or in the form of a folded 8 to stir anti-clockwise. Motor must be tilted a little, to prevent the belt from scratching, when used in an 8 form. You will be surprised what a 2-way stirrer motor costs, this is definitely cheaper to make yourself. A 350 or 500 RPM motor+pulley and a SS-shaft+pulley with an outboardmotor SS-propellor attached is sufficient for all purposes. Instead of this expensive propellor you can design any other SS-mixerblade made by a machinist shop which will do the same job just as good, but will be much cheaper. ^2: Heating such a 1600 liter vessel can be done in various ways, but the best is some sort of coiled-up hard-chromed copper pipe ( do NOT forget to hard-chrome the copper coils at a chroming-shop before ever using them in this kind of reactions, pure copper will solute in 15% sulferic acid and turn your solution to a nasty darkgreen color). Place the coil, or coils, if your man-hole is too small for one big coil, at the bottom of the vessel and connect the ends outside the vessel to a convenient gear-pump and  heating vessel, silicone-oil filled, and electrically heated, with a connection to a thermostate, triggered by a thermometer at the bottom of the 1600 liter vessel. Make the passages through the vessel top airtight with silicone glue! This way you are sure to not form hotspots. Another easy method is to attach electrical heated car motor-oilpan heating pads to the outside of the bottom and eventually the sides of the 1600 liter vessel. This method can be combined with the above one, to speed up heating, do not forget to stirr maximal when using heatpads. 30 August 2001 by LaBTop. WISDOMwillWIN WISDOMwillWIN
	LaBTop (Daddy) 01-02-02 23:49 No 252179		Re: Detailed Methods for Non-chemists .	Bookmark Reply
			Ritter (Master Whacker) 01-02-02 23:26 No 252122          Re: 02 Wacker Help Please   Someone told me that the IPA (isopropylalcohol) 02-Wacker has produced the most consistent yields of 2-propanone (xxx-ketone).  The secret is to warm the reactor to at least 40'Celsius to accelerate 02 absorption to a decent pace.  It has been observed that when this variation is run at room temp, absorption may completely cease long before even half the alkene has reacted-no matter how hard you mix it.  One mole of alkene absorbs over 80% theoretical oxygen in less than 6 hours using an initial pressure of 75psi.  It is very important to use some type of non-metallic  material for the rxn. vessel.  Many people here have wasted thousands of dollars worth the Pd salts over this mistake!  WISDOMwillWIN

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