## On Mishaps & Tragedies in Making MDMA

### by Zwitterion

The road to MDMA is paved with good chunks of broken glass so be careful with your feet! Lately ZWIT has had some SERIOUS FUCKING PROBLEMS trying to scrounge together a batch of MDMA. What was the cause of 8 consecutive failed runs?!?! Why all the wasted methylamine, ketone and time??? What dark and evil conspirators lurked in the shadows waiting to FUCK ME UP THE ASS AGAIN?!?! It was all really quite simple, but the process by which the answer was found illustrates the PROFOUND LACK OF KNOWLEDGE an underground chemist has about the quality of his (and they almost all are HISes) reagents as well as what da fuck he's doing! This tale is possibly the MOST EDUCATIONAL ZWIT WILL EVER POST. Pay the fuck attention, damnit! ZWIT had secured some new space to conduct his operations, and was feeling the old urge to fire up the glassware once again. The minions were getting fiesty, product was running low, demand was high. No better time to satisfy the screaming lunatics among us who LOVE PURE MDMA. ZWIT's product is well known for it's quality among those in the know, and ZWIT NEVER LET'S THE AFFICIONADO DOWN. Or so ZWIT thought. Two batches of isosafrole were made, simultaneously, in a fists of fury tag-team no holds barred fight to the death match. ZWIT vacuum filtered the hot batches and directly distilled to yield an unprecedented 190g of "isosafrole". ZWIT, casual in doing this process, did not bother to actually watch the temperature of the reaction vessels, and in combination with vacuum filtering, introduced TWO VARIABLES into an otherwise solid process. ZWIT should have known that a 95% yield was UNPRECEDENTED and likely NOT the result of filtering, but HINDSIGHT IS 20/20, huh? Error #1 - Two variables introduced in making isosafrole - result: INCOMPLETE conversion of the safrole to isosafrole. ZWIT then started up two simultaneous batches of MDP-2-P at the largest batch size ZWIT's glassware selection could accomodate: 85g of isosafrole processed each. ZWIT was intending on neutralizing the glycol intermediate as per Eleusis's "Improved Method" document, so ZWIT figured a bigger batch wouldn't be a problem (otherwise ZWIT would not be able to distill & concentrate that much volume conveniently). Anyway, things were going NORMALLY, the neutralization went smoothly using 40% NaOH solution, and resulted in a large quantity of the pure glycol ester from each batch. The separate yields of glycol ester were placed into 1L beakers with stir magnets in place, the requisite amount of methanol was added, and as much 15% Sulfuric Acid as could be working on the premise that as it evaporated off over the 3 hour hydrolysis time, more would be added. The beakers were placed in a hot water bath that barely got the core reaction temp up to 75C, but it seemed fine. The smell was different, but ZWIT assumed that this was the result of the "cleaner neutralization" process, as compared to vacuum distillation. So far, in just this process alone, we have racked up 2 variables! Poor form on ZWIT's part! After hydrolysis, the solutions were individually neutralized and extracted with CH2Cl2 (2 more variables, total of 4). The solvent was stripped off, flashed with vacuum to get the last bit out, then the vacuum cranked down hard to 10mm Hg and the "yellow oil" distilled off. the distillation range covered from 120-160C, which is unusually WIDE. Normally the range is 145-165C. The product was the familiar yellow oil, had the "right" smell, etc... If I actually had kept some MDP-2-P from a previous batch, though, it would have been obvious that something was seriously wrong! Error #2 - 4 freakin' variables were introduced into this process! 1) the glycol ester was neutralized with base instead of concentrated under vacuum, 2) the glycol ester was hydrolysed on a water bath which only got the temp up to 75C instead of refluxed in a flask with a heating mantle @ 100C, 3) the post-hydrolysis mixture was neutralized with base instead of extracted & washed and 4) the crude "ketone" was extracted with methylene chloride instead of toluene or ether. The result was a homogenous mixture of the alcohol & the ketone. No surprise then that the Al-Hg reduction failed, then, huh? But the trickies bastard part of this collection of fuckups is that all the errors pointed to a PROBLEM WITH THE Al-Hg REDUCTION, NOT THE INITIAL SCREWUP WITH THE ISOSAFROLE!!! To further compound the problem, a different brand of Aluminum foil was used! The biggest mystery that faced ZWIT was why E & me's process, which had a screaming yeild up to this point, suddenly dropped by 50% while also making a nasty goo which was nearly impossible to crystallize!?!?! My reasoning and deduction process is listed below, substantially assisted by the venerable bastard himself, e. Observations: the almagam reduction gives a 50% yield instead of 85%, the product is oily and difficult to crystallize, a substantial part is lost in the acetone wash, later runs where the freebase was distilled yielded the PROPER AMOUNT OF OIL, the color of the reaction was the same, two layers formed in the flask as usual after vacuum filtering off the oxidized aluminum, the reduction was finished within 3 hours instead of 7, the temperature was unusually easy to control, there weren't too many fumes being made. The strangest clue came at batch #6 when ZWIT vacuum distilled the crap left over from solvent washing the post-reduction, post-concentration mixture. What ZWIT found, not surpisingly, was the alcohol!!! E was totally floored by this, saying that there was no way the Al-Hg reduction could reduce the ketone back to the alcohol, but the proof was there, so we thought! E asked about the ketone, and ZWIT told him it looked normal - what else could E do??? He suggested ZWIT try using plain old Reynolds wrap and see if that corrects the problem. No dice, yield was even worse. All this time, ZWIT was prepping the isosafrole with the same carelessness, and the MDP-2-P without modification - ZWIT didn't want to introduce any new variables! Hah! Finally, ZWIT started to suspect the ketone, and reverted back to the completely normal way of making it - the result? A much more obviously fucked up product! The ketone was definitely wrong smelling and wrong looking, and yield was horrible. Does this mean the improvements E has made to the process are invalid? Not necessarily, but it does mean the improvements MASK THE PRESENCE OF SAFROLE IN THE ISOSAFROLE!!! Having exhausted every other possibility, requiring 8 consecutive fucked up batches to determine, ZWIT finally produced the ketone successfully by MONITORING THE TEMPERATURE OF THE ISOMERIZATION PROCESS THE ENTIRE TIME!!! The isosafrole was then used in the conventional ketone process (ZWIT hasn't gotten around to actually verifying E's improvements with the genuine isosafrole yet) and a side-by-side comparison of the fucked-up ketone with the real ketone showed an obvious difference. The fucked up ketone had a milder smell and was a darker yellow, compared to the pepper-like smell of the real ketone with it's fluorescent green-yellow transparent color. What a tiny amount of difference to detect without side-by-side comparison, though! The final test was doing another amalgam reduction, BUT, ZWIT had run out of reagent grade methylamine so had to use some he made following E's process!! ARGH! Two variables once again, but this time the ending was HAPPY! 34g of MDP-2-P and 38g of the homemade methylamine HCl were reduced to yield 31g of MDMA*HCl doing it completely by the book (Shulgin's book, that is). The product was exceptionally clean, just as expected, and burst into white crystals on the plate when disturbed by a plastic rod. Acetone washing resulted in little improvement in cleanliness (but would have had ZWIT used his improved process of purifying the crude MDMA, which skips the bastard wash & extract steps). ZWIT breaths a big sigh of relief! In conclusion, it should now be obvious that a fuck-up in the first part of the process has monumental effects in the final product! Pay attention! However, it's nice to see that E finally came up with a process for making methylamine that works AND isn't a pain in the ass! Thanks E for saving ZWIT's ass, more than once. I owe yah. [END OF TRANSMISSION]