[enter Tom Robbins Mode]

So you thumb through PiHKAL and stop at synth. 109. Say, it looks so nice, you decide to give it a whirl. Of course, you have already taken your licks learning the chemistry and lab technique, so all that's stopping you is the sheer tedium of the process.

[exit blithering, aimless, Tom Robbins mode]

Alright, today's infomercial-quality post concerns a tricky modification to the work-up of MDMA oil from what The Good Doctor does in PiHKAL.

Old ZWITTERION has had his nose to the grindstone pondering a way to pump up yield while preserving pristine purity in the product - because the only thing more important than a good yield to ZWIT, is a pure yield (of course, the two go hand in hand at the top end of percent yields).

What I wished to accomplish specifically was a way to go from the crude freebase oil/salt mixture which results from stripping the solvents off under vacuum, to the HCl salt of MDMA without all that washing, extracting and extraneous crap. Even more specifically, I wanted to kill that god-awful step where you pour the freebase oil/salt mix into 2 liters of water, convert to the salt, then wash, etc... That step is an OBVIOUS killer on yield, and there are such better ways to get rid of the major impurity, which happens to be the DIMER of MDMA.

Now, at first the obvious route was considered, tried, and found good success with. What's the obvious route? Washing the freebase oil/salt mixture with water to get rid of the salt, then dumping the oil into ether and bubbling HCl gas through it. This gave an exceptional yield of nice white crystals which cleaned up exceedingly well with Acetone.

Yes, Acetone. If you are getting brownish crystals, better wash with Acetone to get them sparkling clean. Pure MDMA HCl is negligibly soluble in it, so all your loss will be impotent contaminants (in other words, don't whine when 20% of your "product" gets washed away as you're product was only 80% pure).

However, the downside to this process is that it wastes a lot of ether, actually takes LONGER to do than the conventional washing, and LOTS of HCl gas is required (read that as: you need a good fume hood, and preferably one that doesn't vent into an apartment complex!).

What's the alternative ZWIT came up with? The natural synthesis of Shulgin's ways and the HCl Bubbling way.

Once you strip off all of the alcohol and amine under vacuum - BTW, it is NOT necessary to strip off the remaining water from the oil/salt mix - wash the two-phase mixture with an equal volume of water to rid the oil of salt. Back extract the wash water with methylene chloride to get any carried over MDMA oil, then combine the back extract with the washed freebase oil. Strip off the methylene chloride under vacuum, then add the crude oil to twice it's volume of 91% (or anhydrous) isopropyl alcohol. Then add enough concentrated HCl until pH is less than 2. Pour the solution out in a thin pool on glass or ceramic plates and heat on a steam bath (use a large boiling pot on the stove with about 1" of water in it) for about 10 minutes each plate. Set the plates aside to cool, and once at room temperature, you should at least see sparse crystallization occuring. Don't worry - all you have to do is start scraping the oil around the plate, with some healthy chopping motions here and there (called "triturating" it) and crystals will spring to life.

Scrape all the crystals into a suitable glass or plastic container and then cover with about twice the volume of Acetone. Swirl, stir and chop well, then decant off the Acetone. Repeat with one more wash, then spread the raw crystals out to dry on a plate. Steam may be used once again to increase the speed. Once all dry, scrape, chop with a razor blade, and weigh.

I have found that one normally gets an amount of MDMA*HCl in grams equal to or slightly greater than the amount of MDP-2-P used in the first place. This is much more inline with what I would expect out of an Al-Hg reductive amination.

Also, speaking of Al-Hg aminations, try conducting your next one in a large Erlenmeyer flask with a stopper in the neck. Run a tube from the stopper into a beaker of dilute HCl to catch methylamine which boils off of the reaction. Then, after several runs, you can evap. the dilute HCl to yield recovered methylamine HCl, as well as totally killing the intense ammonia smell the reaction will otherwise infuse your immediate living space with.

[END OF TRANSMISSION]