Here you go Sneak.
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This reaction is the golden goose, chemists have been hacking away at this forever. You must remember that many of the ratios, concentrations, etc are finely tuned, changing them will drastically change the reaction, which is not always the case. Do not alter the reactions or you will be pulling your hair out.
Safrole: This reaction actually will work with impure oil, some impurities such as eugenol will increase yields by lowering side reactions, this is not true for most reaction tho, just this one. You can use pretty crude oil, no need to distill. Just throw into a sep funnel and wash with an equal ammount of water then wash with an equal amount of ethanol. This should be clean enough to work, just make sure to adjust the amounts if you know the oil still has impurities. Also, certain highly reccomended US vendors have oil which phenolic impurities. These impurities actually help SN reactions and will interestingly enough INCREASE yields as opposed to hurt them.
Setup: For many of these reactions harsh smells/vapors will be produced, the best thing you can do is set up your water aspirator with a hose going down the sink, the surround the hose with a wet rag to prevent any smells from seeping up. Even if the reaction requires normal pressures, its good to run the aspirator on it with an inlet for air, so it doesn't pull a vaccum. This will suck any vapors into the sink water and straight down the drain.
Bromosafrole formation:
Add 190ml of GAA to a flask, then add 75g HBr. The amount of HBr will need to be adjusted because hydrobromic acid is not sold as 100%, usually its sold as 48% constant boiling solution, so a little more than double the amount. Cap the flask with a plug that has 2 holes, one of them leading to your vacuum aspirator, the other you will leave open. Turn on your vac aspirator. slowely add your acid (180g h2so4 100%, it wont be 100%, recalculate for your purity) with a syringe/burret to the solution, there will be foaming and fuming so do it slow. Once all the acid is added get the temperature back to 20C or less and add your safrole/sassafras oil (160g). Give it a few quick swirls then remove it from your aspirator and place in the freezer at around 0C for 24 hours. Don't stir this too hard as you will lose yield, just enough to mix then let it sit. Also don't let it freeze, up to 10C is fine if you don't have a freezer thats in range without being too cold.
Pour off the solution from the freezer into flask A, you are seperating the salts that have precipitated, do this slow and carefully. Do not mix, your compound will get stuck in the salts! Set aside flask A and add water to the solid materials until they are dissolved, then pour this into your seperatory funnel, extracting with either DCM or TCE once, then dumping the aqueous solution. Save the organic (DCM/TCE) layer aside in beaker 2.
Pour flask A carefully into a seperatory funnel also add beaker 2 contents, then add 2x its volume as cold water. A lower layer will form with your product in it (using dcm, tce will be upper possibly). Seperate off this lower product layer into sealed flask B.
Clean your sep funnel and pour flask B containg your bromosafrole and organic solvent. Add 1x its volume as water and then *slowly* add baking soda while stirring with a rod (no shaking here!), keep doing this until it stops fizzing. Once the solution is free of acid seperate the organic layer and throw away the aqueous layer. Put the organic layer back into the funnel and wash it with 1x volume of pure water, then seperate and remove the water. Do this again but wash it with saturated kosher salt water (no halides in the salt, look at the label). Seperate the organics and throw away the water.
The organics need to be removed so you are left with bromosafrole. You can do this by putting in a flask and adding a plug that only has 1 hole with a hose pushed through it, this hose is attached to your aspirator which is run with your water cold and full blast. This will distill off the solvent at room temperature, if you are using something other then DCM or TCE you may need a warm water bath under this flask.
Once this solvent is distilled you have a pure solution of bromosafrole. This must then be converted to iodosafrole in the next step, the Finkelstein swap. Most chemists think that you can use this bromosafrole directly and this is why nobody has really capitalized on this reaction. You must go through the next step and convert it to iodosafrole, this is very important for this method. Even though it is an extra step iodine is a much better leaving group and makes a much cleaner end reaction at standard presssure. If you skip the next step you must do it in a sealed container which is a bitch.
Do not let bromosafrole sit around at room temperature in an open flask. It is stable but it is also volitile so make sure to keep it in a small container and capped.
Iodosafrole - Finkelstein rxn
For every 20g of bromosafrole reacted in the next step, use 200ml of acetone and 13g NaI. Add the acetone and NaI then pour in bromosafrole and let this react at RT with slight manual stirring for ~30 minutes, wont hurt to let it run a little longer. The reaction will end very similar to the first one and will be "worked up" the same by seperating salts, adding 2x water and extracting, extracting the salts, combining extractions, wash (no baking soda needed, just water and brine washes) and then evaporating the organics to get your pure iodosafrole.
So now you have your pure iodosafrole ready to go, time for the next step.
Your crude methylamine.hcl should be prepared by reacting formaldehyde with ammonium chloride.
There is a photowriteup here:
http://www.erowid.org/archive/rhodium/clandestine/methylamine/index.html There are some things to improve the process. Do it in a container which you can remove the crude MeAm.hcl from after the process. Instead of using a hotplate/etc what you need to do is get a large container that will fit your flask, add enough water to come up to the liquid level in the flask, not above it. Boil this water in the bath and keeping adding table salt to the bath until the solution is super saturated and does not hold any more. This solution will now boil around 105C constantly as long as the water level is kept steady. During the process you need to hook up your flask to your water aspirator, turn the water on low so that during the process there is a very low amount of bubbling, like carbonation rising. Not bubbling hard, just a little tiny bit. Follow these steps and you will have some very pure crude MeAm.hcl for the next step. Once the reaction has run its course
Last Step:
For this reaction you will be freebasing methylamine.hcl to release methylamine gas into isopropyl alcohol. You are going for a 20%+ concentration by weight of methylamine gas in dry IPA, higher concentrations will mean a better rxn. The methylamine must be present in 10-15x molar ratios, 10 being the bare minimum. For 200g iodosafrole you will need around 300g methylamine gas dissolved in 1500ml of dry IPA. So I would start with freebasing around 400g crude MeAm.Hcl from earlier to be safe. This will require about 300g of sodium hydroxide dissolved in minimal water to freebase it. You should add around 100ml of water to a stainless steel pot and then add your sodium hydroxide, this will get pretty hot, use the heat and keep adding water until most of the NaOH dissolves. You need to heat the water to get more than possible sodium hydroxide dissolved in it for the next step. If you use the bare minimal amount of water then you do not have to dry your meam gas, which logistically helps a lot. You then load this into a syringe and add it to your crude methylamine.hcl to create methylamine freebase, a gas, which is then bubbled into dry IPA. You should weight the IPA container before adding the gas, and then weight it afterwards to determine how much was absorbed.
Once you have your crude methylamine, scoop the correct amount into a flask to make a meam gas generator and install the 2 hole stopper. In one hole you will have a large 50ml syringe for adding your base solution, in the other a hose with a basic suckback trap, don't bother trying to dry the gas like many do, it will only cause problems and pressure buildups. I would use plastic tubing which is thinner than .25", the thinner the better. At the end of the tube place a loose ball of glass wool to make a disperser which wont cause a lot of back pressure. Between the end of the tube and the reactor you need a suckback trap. This is made by making another 2 hole stopper and placing it in a tiny flask. When the temperature of a reaction that produces gas changes there is a rapid suckback effect, this will happen once your reactor ceases to produce the gas and it cools down a bit, if you do not add a trap you could lose product. Place the tube straight into the IPA flask.
Cool the IPA in the IPA flask in freezer on the lowest setting then add a 3 hole stopper. 1 hole the gas tube from the suckback is inserted through, the other hole goes to the vacuum aspirator and the last hole is kept open. Its very important to leave this hole open, you can loosely stuff a wet paper towel in to prevent smell from coming out, but it needs to be open for safety, this reaction is run under negative pressure anyway so fumes wont pour out of the hole. Turn on your water aspirator on the lowest setting, just enough to clear fumes from the rxn. Use the syringe and suck up the first part of your super saturated naoh solution in the syringe and drop it into the crude methylamine slowly, at a rate which you can not smell the methylamine coming through the hole in the 3 stoppered flask. Once the correct amount of methylamine gas has been added by weight remove the 3 hole stopper and quickly add your iodosafrole, then insert a stopper with no holes. Its a good idea to tape the stopper onto the neck of the flask. Shake this around with a gloved hand, you should see a very rapid color change. Let this sit in the ice bath for 30 minutes to make sure it has totally reacted, then under good ventillation and being careful, slowly release the pressure on the flask and remove the stopper, add a 1 hole stopper and a tube going to your aspirator. Place the flask into a room temperature water bath and let the water aspirator distill off the methylamine and some alcohol. You know when its done when it no longer smells like rotten pussy fish. Pour this solution into your seperatory funnel and add an excess of 10% base solution. Once your base has been added a nice yellow/golden oil will fall to the bottom, seperate this and extract the rest of the solution with toluene/xylene, around 100ml per 10g expected yield and add this xylene/freebase to your golden oil. You can then either titrate the freebase solution with HCl solution or gas it in the standard way. There are two options depending on your situation. Titrating requires a distillation setup but it works better on the large scale, wetness of the solution is not as big a problem. Gassing is less materials intensive with simple equipment but requires drying and works better on the XXg and XXXg scale.
Titrate: To titrate the solution place your xylene/freebase solution in a flask. Use 15% HCl and add it dropwise until the ph goes from 10+ to around 6. Once you added enough acid then distill off solution until the flask does not look wet. As you distill off xylene water goes with it as an azetrope, toluene works better in this regard. You keep distilling the solvent until it looks like all the water is gone, this will be very obvious if you pay attention to the sides of the flask and the condensation, wet looking effect wet solutions have. At this point cap your flask and put it in the freezer, crystals will form inside of the flask, drain off the xylene. Titration tends to be dirtier than gassing so you may need to recrystalize.
Gassing:
A cup of epsom salts is microwaved while grinding every few minutes until it all looks dry and white, no longer clear. This is dehydrated epsom salts, very hydroscopic and can not be stored, must be made day-of. It is hammered to powder it a little. A few rocks are placed into a large plastic funnel to provide a flat base and then a filter paper is placed over it. The warm dry epsom salts are poured into the funnel providing a layer atleast 1.5 inches thick. This is placed into a small hole in a bucket, which is placed so that the seperatory funnel drips directly onto the filter and into a dry bucket. Once this xylene has been filtered it will be a very clear orange solution, ready for gassing. If its cloudy dry again or else you will slay your yield, so drip dry it slowely the first time. MAKE SURE IT IS CLEAR OR DRY AGAIN. Once you have this clear solution in a bucket set up a HCL gas generator
This is done by placing about 1kg damprid in a flask with a stopper which has a hole for tubing. Add 20ml of muratic acid at a time to the flask and quickly replace the stopper. As liquid hcl hits dry hcl gas will flow, pipe this into your DRY xylene/freebase solution and mda.hcl will precipiate, keep filtering whenever you are between gas flows from HCl addition. If you want you can skip filtering until the end but this way its easy to tell when the reaction is over, no more crops of crystals will appear.
Cleanup: Not usually needed unless you want to grow huge, clean, clear rocks or used the titration method
This method is called a dual solvent recrystalization, this has been done if your molly is a fine sand, not fluffy powder or small crystals:
First you need a large stainless steel pot, in this pot put your molly. Add either pure methanol or 99% IPA slowly until it is all dissolved. If you go overboard and add too much alcohol then you will just need more acetone later and it becomes wastefull, so add it maybe 20mls at a time. IF you have good ventilation and want to use less materials then you can let the alcohol boil while it dissolves the molly, you can use like 25% of the alcohol this way. Anyway depnding on your purity and alcohol temperature you should have around 1L to 3Ls of yellow/organge/brown molly alcohol solution.
Now you need some acetone, use 4x the amount of acetone as you have molly alcohol solution. To answer your questions there is really no difference between hardware store acetone which has been dried and reagent grade acetone. Actually ordering a large amount of high quality acetone is one of the more suspisious things you can do when it comes to chemicals suprisingly. You can dry the acetone by adding about a cup of calcium chloride (DampRid) from the hardware store per gallon of acetone. Let this sit for a day and pour off the acetone leaving the solids at the bottom. You dont want to use mgso4 with acetone, there may be minor reactions that go on. Anyway its a good idea to dry the acetone but not necessary for fresh hardware store acetone which has been stored correctly.
So what you do is have a jug of the acetone with a stirring rod, stir the acetone and add the alcohol solution to it, you can do it all at once then stir but its better to do it slow and i will explain why. The reason this method is so good is because when you acetone boil the molly there are still impurities in the crystal structure, dissolving in this way allows those impurities to go into solution, dripping the alcohol molly into acetone causes the crystal to reform, but this time as very fine poweder with acetone all around it. the slower you do it the cleaner it will be, but it can be done all at once. Once this is done cover, seal the container airtight and put it in the freezer, it must be air tight or moisture will leak in and lower your yields. When the liquid is ice cold you should recover your molly by clamping an old tshirt over a bucket, and filtering it. Then you can just put on gloves and twist the tshirt molly package around to compress it and let the juice out. Another way would be to get an apple juice carboy, drill a hole, add a hose barb and attach that to a water aspirator on your sink, then you can put a large buchner funnel on top and have a vacuum remove the liquid/dry it out. But the tshirt method and then spreading it in a thin layer is good enough.
Growing Moonrocks:
for 10g mdma use 250ml acetone, place the mdma in the acetone, it will not dissolve. carefully heat the acetone to almost boiling (dangerous fumes) and slowly stir and add water dropwise SLOW. When all the mda dissolves in the solution very slowly cool it. The slower the sexier the moonrocks.
Don't know why a route guide that's such common knowledge here needs to be deleted...
is that a joke? The sulfuric is only needed when making hbr in situ with nabr in gaa.