Author Topic: thiol-ephedrine/urshibira Ni redux  (Read 899 times)

0 Members and 1 Guest are viewing this topic.

stratosphere

  • Guest
thiol-ephedrine/urshibira Ni redux
« on: December 27, 2003, 06:58:00 PM »
I couldn't find anything in TFSE about this specific method, but in concept it seems straight forward, and the materials are easily available.
the only real Downside is H2S generation so  some sort of make shift fume hood would be needed.
Basically the idea is to take advantage of the fact that thiols are very easily reduced catalytically.
So just to give a sketch of  what im invisioning:

First make chloroephedrine by combining ephedrineHCl, an excess of HCl and some ZnCl2 catalyst and heating in a sealed bomb.
(there are notes in the index about making chloroeph)
after that the excess HCl is killed with sodium-bicarb.

Separatly and in a fume hood a solution of NaSH is produced (moles of NaSH=moles of chloroeph) , additionally one mole of Na2S must be added for every mol of ZnCl2 used.

This is added to the chloroeph soltn to yield thiol-ephedrine, with ZnS precipitating, filter out the ZnS and give it to your mother for Christmas, but save liquid thiol-eph soltn.

Next urshibira nickel is prepared, im sure there are figures available for how much hydrogen gets trapped versus how much Ni/Al etc you use. I would say first figure out the minimum you need based on that (mols of trapped hydrogen= mols of thiol-eph), and then double it because having too much will not hurt anything, but having too little will.

Use a drop funnel to drop the thiol-eph onto the urshibira nickel. When it gets reduced it will make H2S, so its very important that its done in a hood, and that there is a hose leading from the top of the urshibira nickel flask being bubbled into a flask of  concentrated NaOH solution so as to capture the h2S as Na2S.

After a bit of workup (filter out Ni, standard polar-nonpolar acid base extraction) you should have some grade A government anti certified meth.