Stuff you’ll need:

Stuff you’ll need:

The recommended amounts below allow for a bunch of mistakes. Believe me; you’ll make them. I started with a quart of sassafras oil, just to give you the scale, and used about 2/3 of it.

Chemicals:

• Sassafras Oil: this is about 80-90% safrole. Look for aromatherapy supplies. You can get it on the web. Be sure to get 100% sassafras oil — don’t get it mixed with anything else. It’s about $45 per quart, and a quart is vastly more than you’ll need, but I’d get at least a half quart (I guess that’s a pint).
• MeOH (methanol, wood alcohol): I got mine from a lab supply house, technical grade. I’d get a gallon or two to account for fuck-ups. Maybe you can get it at drug stores, but all I’ve seen there is denatured ethanol and isopropyl alcohol. I eventually used two gallons.
• Distilled H₂O: Distill it yourself, or get it at the grocery store. You’ll need a few gallons (perhaps 5 or 6) by the time you’re done. Get distilled water, not “spring water” or some other such shit.
• p-Benzoquinone: Get this from photography supply shops. I got a pound and had plenty for a lot of trials.
• Palladium(II)chloride (PdCl₂): Photography supply shops. This is expensive stuff ($25/gram). I got 5 grams total. Get exactly this — not a replacement or a mixture of this and something else. You can do it 1 gram at a time, but the “recipe” below calls for 2. If you only have 2 grams, do two 1-gram batches.
• DCM (methylene chloride; dichloromethane): I got it from a chemical lab supply house, technical grade. I used less than a gallon.
• Xylene: Chemical supply house. I used technical grade, and eventually went through an entire gallon.
• Acetone: It’s with the paint thinners in a hardware store. I got a gallon and it was more than enough. Mostly, I used it to wash and dry glassware, but you also need a little bit for the final wash of the sacred chemical.
• NaCl (non-iodized table salt): grocery store. Be certain it’s not iodized. I don’t know what the iodine would do, but I have a healthy imagination, and none of the things I could imagine were good. I think almost all salt (maybe not kosher salt) contains sodium aluminum silicate. Mine did, and that didn’t seem to cause any problems. It’s cheap — get three pounds.
• NaHCO₃ — Sodium bicarbonate (baking soda): grocery store. One big box is plenty.
• NaOH (lye): I used Red Devil lye from a grocery store (drain cleaner). Get pure, dry lye. Not Drano with the little aluminum flecks, or anything that’s already dissolved. Get three or four cans of the stuff.
• HCl (hydrochloric acid, muriatic acid): Get this from a pool supply place. I got a gallon, and it was far more than enough. It’s cheap. Get a gallon or two.
• MgSO₄·7H₂O — Magnesium sulfate: These are epsom salts. Get them at a drugstore. You’ll need to cook it to get rid of that “·7H₂O”. I bought the amount that fits in a container that’s the size of a half-gallon milk carton.
• Nitro RC fuel: From a hobby shop that sells fuel for the RC models. I got a gallon for around $30, and it was far more than I needed. Get the highest concentration you can. The best I found was (supposedly) 40%. It’s a mixture of nitromethane, methanol, and something like castor oil. I hear that even higher concentrations are available. The kid that sold me the 40% stuff seemed really concerned that I’d ruin my model airplane engine using such a high concentration. I assured him that I’d dilute it with some methanol — yeah, right.
• Aluminum foil: I used the “extra heavy duty” Reynolds wrap. One roll from the grocery store is plenty. Apparently the stuff called “heavy duty” also works, but I assume the reaction will run faster (and hotter and scarier) with it. Everybody cautions against the regular foil. It is just too thin, and believe me, you don’t want to see that reaction “run away”. It barrels along at a pretty heart-stopping rate even with the extra heavy duty stuff.
• Peanut oil: Grocery store. Get a couple of quarts.
• Safflower oil: Grocery store. A little bit; all you need is a few ounces. Be sure to get the stuff with NO ADDITIVES since it’s going to get hot and be mixed with something you eventually eat!
• HgCl₂ (mercuric chloride): From a photo chemical supply place. You don’t need much — 3 or 4 grams is plenty. I think I got an ounce and used only a tiny amount. Maybe there’s some way I can feed the rest to certain politicians. Careful: this stuff is REALLY poisonous.
• Sulfuric Acid: I used the high-powered drain cleaner. I got it from a hardware store. I used less than a quart. I don’t need to say “be careful”, do I?
• CaCl₂ (Calcium chloride): I used “Damp-Rid” that I got from a hardware store. It’s with the mildew prevention chemicals. One cannister is plenty.

Apparatus:

Be sure it all fits together. I used 24/40 connectors throughout. The 24/40 seems to be the most easily available stuff, and it seems quite suitable for the quantities of chemicals you’ll be using. If you already happen to have larger or smaller stuff and just need a piece or two, go ahead and use that, but if you’re starting from scratch, get the 24/40 size.

If you haven’t done this sort of thing for awhile (or ever), obtain a manual on organic lab techniques. Read through the appropriate section before you begin using any technique. Of course you’ll screw up anyway, but this way you’ll screw up a couple of fewer times. The manual recommended by many illicit chemists is this: “The Organic Chem Lab Survival Manual “, by James W. Zubrick. Others work fine, too.

For me, at least, it was critical to have something like the “CRC Handbook of Chemistry and Physics” or the “Merck Index” to look up physical properties (especially boiling points) of such things as methanol, acetone, safrole, eugenol, …)

Glassware:

• 1000 ml 2-neck round-bottomed flask (RBF)
• 500 ml RBF
• distillation head
• vacuum adapter
• thermometer coupling
• vigreaux column
• distillation column
• separatory funnel: at least 1000 ml — 2000 or 4000 ml is better.
• addition funnel: at least 100 ml
• 2000 ml two-neck RBF (not required, but nice)

(If you’re lucky, you may be able to find a separatory funnel with a 24/40 fitting at the end that you can use as an addition funnel as well. I was not lucky, so became the proud owner of yet another piece of glassware.)

Other Stuff:

• Buchner filter, filter flask, flask stopper, filter paper.
• Coffee filter + filter paper
• Combination hot plate/stirrer. You can’t get away without this, especially for the final step, and it makes life a lot easier if you have it at the beginning. I got mine late and was sorry.
• Magnetic stir bar (get one that’s egg-shaped and works in RBFs)
• Clips to hold the glassware together.
• Two lab stands and at least two clamps. Don’t skimp on the clamps — they hold hundreds of dollars worth of glass!
• Aquarium pump (to pump ice water through distillation column)
• Thermometer that fits coupling (0-300 degrees). It’s nice to have two — one to watch the temperature of the stuff that’s coming over in the still, and another to check other temperatures, like the temperature of the peanut oil, or of the fluid that you are distilling.
• Boiling stones. You can often avoid using these if you’ve got the hotplate/stirrer. The spinning stir-bar works better than boiling stones under vacuum conditions, since there tends to be a lot less “bumping”. If you’ve never seen bumping, let me tell you a secret: the first time it happens to you, you’ll be very upset.
• Silicone grease
• Vacuum pump. I used a spa pump with enough pipes to take water out of and return it to a 5 gallon plastic bucket.

I attached an aspirator to this.

• Plastic tubing (3 pieces — two to connect to the input and output of the distillation column; one to connect the aspirator to the vacuum adapter, or to the flask holding the buchner funnel). Make sure they’re long enough. I used 2 sections that were about 2.5 feet and one of 6 feet.
• Measuring cups and/or graduated cylinders. I used a 500 ml cylinder plus a 50 ml cylinder.
• Triple-beam balance.
• Glass wool (I got a furnace filter and cut out chunks of the wool). I used it to plug the vigreux column when it was filled with glass beads and calcium chloride).
• Lots of clean glass jars for storage. Next time I’d just get a dozen mason jars (quart size) with lids. Some smaller jars are good, too.
• Tiny spatula for measuring out tiny amounts of dry chemicals.
• Glassware cleaning brushes. Get at least one curved one for cleaning the insides of the round flasks, and one straight one.
• Glass beads to fill the vigreux column for fractional distillations. The people at the hippie store that sold all sorts of psychedelic colored beads thought it was pretty strange when I looked over everything and finally selected the ugliest (and of course cheapest) beads for my “creation”.
• Coffee grinder (to ball up the aluminum foil) Please clean out the coffee grounds first, and PLEASE clean out the aluminum dust afterwards.
• (optional) paper shredder (to shred aluminum foil)

Synthesis notes

(All temperatures below, unless mentioned otherwise, are centigrade.)

Overview:

1. I distilled sassafras oil to make safrole.
2. I distilled RC model fuel to make nitromethane.
3. I used the Wacker reaction to make MDP-2-P from the safrole.
4. I made MDMA from the MDP-2-P and the nitromethane.
5. I took the ecstasy. This step was more fun than all the other steps put together!

Safrole:

There seems to be no problem with the distillation of the safrole from the raw sassafras oil using Bright Star’s recommendations.

If a ¾ horsepower pool pump is used, it appears that the temperature at which the safrole comes over is about 106-107°C on the first pass. For the second pass, I used a vigreux column in addition, and the safrole came over at between 94°C and 99°C. Good vacuum! The pump basically recirculates water through an aspirator as fast as it can using water in a 5 gallon plastic bucket. To get a higher vacuum, there was always ice in the bucket. Thus the temperature of the recirculating water was always 0°C (unless I ran out of ice).

There are a couple of photos on the web of designs for good vacuum pumps that recirculate water. I mounted my pump to a board and then attached pieces of PVC pipe to make an output that sprayed into the bucket, and an input that sucked water from the bucket. I did not, therefore, need to drill any holes in the bucket as was proposed in at least one of the web designs.

The suction also seemed to be vastly better if there was a baffle in the plastic bucket to keep the air bubbles from getting sucked into the input of the pump. I used the lid of the bucket as a baffle and crammed it down vertically between the place where the water from the aspirator fixture sprayed in water/bubbles and the input pipe from the spa pump sucked it out. This uses ice very quickly — without ice, it’s amazing how fast a ¾ horsepower motor heats up 4 gallons of water. By the way, a ½ horsepower motor should be sufficient; I just happened to have one rated at ¾ horsepower.

Also, always run ice water through the distilling column, either when distilling or when you’re using it as a reflux column.

Distilled the sassafras over peanut oil in a 1000ml flask in 2 passes. The result was about 700ml of safrole from 1 quart of sassafras oil.

Nitromethane:

Bought nitro fuel for RC engines at a model hobby shop. The bottle said it was 40% “nitro” (= nitromethane), but after my distillation, I doubt it. It seemed to be at most 30%. Had to do a fractional distillation using a vigreaux column. The fuel is a mixture of methanol, nitromethane, and castor oil.

Note by Rhodium: This discrepancy is probably due to the fact that methanol and nitromethane forms an azeotrope. First a 92:8 MeOH/MeNO₂ mixture (bp 64.5°C) distills over (close to the boiling point of pure methanol, bp 64.7°C) and when all the methanol is gone, the temp shoots up to ~100°C, where pure nitromethane is collected.

Nitromethane boils at 101°C, so I had to do it over cooking (peanut) oil instead of water. It seemed to come over at about the right temperature, but it’s OK to have a mix of the nitromethane and some methanol, since the only time the nitromethane is used is in a mixture that uses methanol as a solvent, and the total amount of methanol is unimportant, so some extra is OK. If there is some methanol, however, it may be important to add a bit of extra nitromethane/methanol to be sure to get enough nitromethane, since that’s critical to making the final product. I used about 10% or 15% more of the mix for that final step and didn’t have any problems.

What I did was to distill for a long time to get almost all of the methanol out, and then, when the temperature spiked up to near 100°C, I let that run for a few seconds, then switched to a new flask to get the nitromethane.

Did I mention that this distillation scared the shit out of me?

What frightened me about the nitromethane is that the Merck Index says that it has a “flashpoint” at 112°F. I don’t know what a flashpoint is, but I didn’t want to find out! Nitromethane is the “nitro” in “nitro-burning dragsters” — you know, those drag-racing cars with all the flames coming out. Note that the flashpoint is far below the boiling point (about 101°C) of nitromethane.

Note by Rhodium: This is not something of concern. The flash point of a substance is simply the lowest temperature at which you can ignite a substance. Gasoline has a flash point at several tens of centigrades below zero for example. It does not mean that the compound will spontaneously ignite or detonate, just that you should avoid sparks or open flames (which is a good rule at all times in a lab).

I tried to distill with a vacuum, and it was very difficult with boiling stones, since there would be a huge “bump” as a huge chunk boiled at once, which reduced the pressure, which had to build up for another huge bump. I did not have my hotplate/stirrer at the time, so I couldn’t tell exactly at what temperature it was boiling, and the temperature was all over the place. Next time (if there is a next time), I’ll try the vacuum distill, but with the stir-bar twirling like a dervish, and I’ll use a vigreux column crammed with glass beads for a good fractional distillation.

Note by Rhodium: Distillation of nitromethane at atmospherical pressure is not inherently dangerous as long as you aren’t distilling it all to dryness. It is not practical to vacuum distill nitromethane, as there is too much loss of product down the drain (using an aspirator as vacuum) or into your pump oil.

MDP-2-P (the “ketone”):

Used Methyl Man’s “Benzoquinone Wacker Oxidation of Safrole in Methanol”.

I tried the long-term stirring of the PdCl₂ in methanol for 6 or 7 hours before adding the water and the p-benzoquinone. You can get the p-benzoquinone and PdCl₂ from photography supply places. I mail-ordered mine from a Canadian lab (I thought this was great, too, since I’ll bet the DEA has a harder time looking at Canadian lab records). PdCl₂ is expensive — like $25 per gram.

I never needed to add heat — just a slow addition and then a long wait afterwards (8 hours to be sure everything reacted). Stirred the whole time.

I used gravity filtration in a coffee filter to get rid of the hydroquinone, and then put the filter in a zip-lock bag and squeezed it to get out the last drops.

When I washed with the sodium bicarbonate, I had a lot of crud on the interface between the DCM and the methanol fractions, but it was workable. The saturated NaCl made a real mess — emulsion-like that just wouldn’t separate. I finally froze it to break it up. I only did one NaCl wash since it was such a pain. Maybe it would be better not to shake the mixture so hard in the separatory funnel. Or maybe it would be better to use distilled H₂O for the mixes. Or both. Next time, I’d use only distilled H₂O for every place I need water, and I wouldn’t shake so hard on this wash.

I did distill in two steps — DCM over water without vacuum, then the MDP-2-P under vacuum over oil. Did it with a stir-bar and it worked OK unless I lost vacuum. Stir bar works much better than boiling stones, especially under vacuum.

I had problems cleaning the RBF afterwards, due to some charred shit. I read later that the best way to clean this is to add some paint thinner (mineral spirits) and clean with that FIRST, before you try stuff like soap and water (and strong acids, strong bases, et cetera). I do know the mineral spirits don’t work so well afterwards…

MDMA:

Used Methyl Man’s “Reductive Amination of MDP2P with Al/Hg + Nitromethane”.

The reason I used this approach is that I was totally unable to make the methylamine hydrochloride (methylammonium chloride, MA.HCl) by any method. I tried BrightStar’s method, as well as about 4 other methods I found on the web. In all cases, I was able to make what were probably mixtures of MA.HCl and ammonium chloride, but I couldn’t figure out how to assess the purity. I also didn’t have any luck getting the stuff I needed to do a purification: absolute ethanol is difficult to obtain; in California, the best you can purchase at a liquor store is about 75%, so you’re faced with a distillation even to get to 95%. Then you’ve got to get some anhydrous calcuim oxide, and I didn’t know how to do that. I even made a bunch of chloroform to clean out other impurities (which you should do), and that was a pain in the butt and perhaps a bit dangerous, too.

The problem is that the ammonium chloride will cheerfully react by the same mechanism as the MA.HCl with the MDP-2-P, but it will make MDA in place of MDMA. I would not have minded a mixture of, say, 3% MDA and 97% MDMA, but I just didn’t know what I’d get. Anyway, the method described below worked perfectly, and should make exactly 0% MDA and 100% MDMA.

At first I didn’t have a 2 liter, 2 necked RBF, so I did half-batches in a 1 liter flask, and that worked great, except that it took, of course, twice as long. There was never a problem with run-away reactions, and I always got a happy result. The full version is a little more tempermental, left more aluminum junk, but worked fine, too. Do this reaction at the end of the day, and let the final stuff sit around all night to make sure the reaction is complete. If you try to do it after just, say, four hours, there will be some aluminum fragments that are still bubbling in the NaOH, and these are a real pain in the butt during the separations. Wait overnight and everything is cool…

I used not only heavy aluminum foil, but the “Extra Heavy Reynolds Wrap”. You can just cut 3 inch strips from the roll and put them through a paper shredder (to make pieces that are 3 inches long and ¼ inch wide) — this is much easier than cutting them by hand. You’ll have to do some dicking around with the coffee grinder to figure out how much of the foil strips can go in at once and not jam the machine. Even with the paper shredder and coffee grinder, it takes surprisingly long to make enough little foil balls to run the reaction.

After the reaction, I poured the grey sludge into large (gallon-sized) bottles, and added the xylene (xylene works fine instead of toluene, by the way) to the bottle. Then I did all the shaking in there before pouring the stuff in a separatory funnel.

I tried the washes with tap water and there was always a lot of gunk. On my final pass, I used distilled H₂O in all steps and things were MUCH better. The moral: use distilled water, don’t use tap water!

When you are drying the epsom salts (do this well ahead of time), don’t put too much in the oven at once. I put a thin layer on a sheet of aluminum foil and cooked it very hot (400°F) in an oven for an hour or so. I made a bunch of batches and kept them sealed tightly in a jar. I also ground the stuff to a powder using a mortar and pestle. I might try a coffee grinder next time. Don’t try to cook up too much at once — this can make a horrible mess.

I used a hair-dryer to dry the bottles that were to contain the anhydrous stuff (after the acetone wash, of course).

I had two bad experiences with HCl generators before I figured out how to do it. This is the way: Add NaCl (lots, non-iodized) to a two-necked flask. A big one (2 liters) is good. Wet the NaCl with HCl, but not too much (no puddles).

Plug a vigreaux column with glass wool (cut from a heater filter), and pour the column full of CaCl₂ (Damp-Rid pellets). Then put the thermometer adapter with a tube instead of a thermometer mounted in it into the top of the column.

Into the other neck of the main flask, put in an addition funnel with concentrated sulfuric acid. All joints should be greased with silicone lubricant. Drip in the H₂SO₄, and anhydrous HCl gas comes out the tube. Do this outdoors — you’re going to get clouds of HCl gas, which you certainly don’t want to breathe. Use the silicone grease throughout.

Even at the end, when I thought there were no longer any mistakes to make, I screwed this up. I tried to powder the CaCl₂ to get better surface area, and then tried to pump through too much HCl gas too quickly. The powder was too fine, it plugged the gas, and finally a giant belch of gas, H₂O, and CaCl₂ was dumped into the xylene and it totally fucked up the batch. TAKE IT EASY AND SLOW WITH THE GAS GENERATION. You have plenty of time, and it’s the last step.

TEST THE TUBE AND EVERYTHING IN XYLENE BEFORE YOU TRY IT FOR REAL! I found, to my horror, that the “aquarium rock” that I added to the end of the tube to make lots of tiny bubbles dissolves in xylene. I had great success with nothing but a hollow tube.

Don’t be a pig — when you get a bunch of precipitate, run it through the filter and then re-gas. It’s even better to chill the xylene mixture to drive out more precipitate. At some point, usually after about 3 gassings, the stuff in the xylene starts getting a yellow tinge and then starts to stink like HCl (maybe water in the xylene?) Anyway, I did it in three passes, and as soon as I saw a tiny amount of yellow, I quit. You can use the slightly yellowed stuff — wash it with acetone, but the more yellow and the more stink, the more of the real product seems to disappear and be dissolved in the water.

When you get the final stuff — MDMA mixed with xylene — get as much xylene as you can out of it on a vacuum filter (returning the xylene, possibly, for another passing of the HCl gas). Then, over the vacuum, put in a few jolts of acetone. This dissolves not only the yellow crap (if there is any), but tends to pull out the xylene and things dry quite rapidly.

I got (on the time I made the fewest errors) about 18 grams of MDMA (dried from the acetone) from 25 ml of ketone.

I did not recrystallize this “raw product”, since it looked snow-white to me. It does have a faint odor (safrole?) but very faint.

Note by Rhodium: Even if your product looks pure and snow-white to you, please do yourself and your friends a favor and recrystallize the product. A lot of unhealthy byproducts are white/colorless just like pure MDMA, so visual inspection cannot be used to verify purity (you can only verify the presence of colored impurities). Pure MDMA·HCl is odorless, so using your nose is a better way to gauge purity.