I watched the crazy old man with the dark trimmed glasses go at it again. This time he fucking amazed me! I saw him do something like 125ml MeOH, 25mL H2O, pinch HgCl2, stirred. 8.9g Al, stirred ~20 mins. Added 6.4g isosafrole ketoxime, added 25g HOAc. ~3 hours pass with mag stirring (flask is only warm to the touch). Slowly added 90g NaOH dissolved in 200mL ice-water. Extracted with 80ml, then 45ml toluene. Washed with 150ml 5% NaOH, filter, 150ml 5% NaOH, 150ml brine. Titrated to pH 4 with HCl in distilled water with stirring. Evaporated water. 5.9g MDA.HCl yield (before recrystallization). (83% crude yield!!!)
The reaction ran HOT and FAST. It was over and done in about two or three hours. The yields are FUCKING STELLAR.
Antibody gets two thumbs up for this procedure!!!
Things learned (this is his third run of ketoxime reduction, btw):
1) you can use MeOH instead of EtOH, which is good news
2) you can amalgamate all the Al before hand and in situ as MM does (very good news!)
This definitely paves the way for OTC MDA.HCl in high yields! (or is it really MDOH.HCl? ahh, who really cares!)
HAPPY, HAPPY, JOY, JOY!!!!!
Btw, the bioassay on the MDMA that the man produced that I wrote about in other posts was predictably good.