I've been looking over Chromic's peracetic writeup at Rhodiums. https://www.thevespiary.org/rhodium/Rhodium/chemistry/peracetic.chromic.html (https://www.thevespiary.org/rhodium/Rhodium/chemistry/peracetic.chromic.html)
In it, he's got the sections called "Typical run reductively aminating MDP2P to form MDMA.HCl" And he says that he adds the HgCl to the Al, and waits 'till he sees a faint bubbling, then adds the methylamine solution along with the MDP2P.
1. So is this all wholesale, just dumping it in, and adding the condensor?
2. Could yeilds be improved by making the methylamine solution with methanolic or ethanolic NaOH or KOH and MeAm*HCl, then adding the MDP2P dissolved in alcohol, and letting sit over night, maybe chilled, before it's put through the amalgum? My thoughts are that if someone could get 78% yeild y just dumping everything into the flask that's already got a running amalgum going, without giving the imine any time to form beforehand, could yeilds be drastically improved by taking steps to form the imine completely? The only other major product of the Al/Hg is MDP2Pol, which is no doubt formed by the ketone being reduced before it has a chance to form the imine. Am I far off on this? Has anyone tried to let the imine form separately before they ran the Al/Hg?
Post 440288 (https://www.thevespiary.org/talk/index.php?topic=11864.msg44028800#msg44028800)
(Barium: "PTC - imine reduction", Novel Discourse)
Please read the last lines from the Notes also. LT/