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/I
2.
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/I
2. (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 107771 (missing)
(smokemouth: "LaBTOP/Gyro performic results - Sumerian", Methods Discourse) LaBTOP-Gyro performic results - Sumerian .
2.
Post 107780 (missing)
(smokemouth: "LaBTop/Gyro's Modified Performic Questions - Synthia", Methods Discourse) LaBTop-Gyro's Modified Performic Questions - Synthia.
3.
Post 107770 (missing)
(smokemouth: "New Performic Scale Up Question? - artech", Methods Discourse) New Performic Scale Up Question - artech.
4.
Post 107739 (missing)
(smokemouth: "The correct way to mdp2p via performic - gyrogearloose", Methods Discourse) 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.html
NaBH4 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.
~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~
~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~