Salting Pure Freebase Harmaloids

[amor_fati]

Not sure if this has been discussed or not. As far as SWIM can tell, the current method relies on salt-water, which is all well and good but may not result in a very pure product due to salt contamination. As SWIM understands it, the freebase form can be incredibly pure, so SWIM has a proposal for converting this back into a hydrochloride without the risk of salt contamination. The inspiration for this idea comes from a certain wizard, named Le Junk:

-Prepare a solution of one part 36%HCl (muriatic acid) and three parts 95%Ethanol (everclear).
-Dissolve freebase harmaloid in acetone (20ml per gram? SWIM is unsure if it will dissolve, please correct him if he is wrong).

Now this is where it gets tricky, as the tek was create for a different alkaloid and had the amounts measured perfectly. It called for twenty drops of the ethanol-HCl to be added to 10ml of fresh acetone. It then called for both the acetone/ethanol-HCl solution and the freebase/acetone solution to be swirled and then combined. This would produce instant precipitation in the case of the intended alkaloid.

SWIM believes that the results would be much the same with harmaloids unless the freebase is is insoluble in acetone or the hydrochloride is soluble in acetone. Anyway, this is merely a proposition that SWIM is currently unable to test, but if it sounds doable to others, he will work toward attempting it.

Also, SWIM was wondering if the conversion is even necessary, or if the freebase sits well enough. SWIM cannot handle swallowing freebase DMT, so imagines that freebase harmaloids would be much the same.

 

[Infundibulum]

Very interesting! SWIM's FOAF has found that freebase harmaloids are indeed insoluble in acetone but he has observed in a single occasion that the harmaloid salts may convert to the "evil" harmala red using a similar procedure.

Now everybody do not take this thing too seriously, it was a single observation that was NOT repeated and it was FREEHANDED.

What this guy did was to freebase harmaloids from Manske using the calcium hydroxide paste, pulled them with acetone when the paste was dried and salt them in acetone using FASA. Quickly precipiitations of the fumarate salts formed in the acetone....WHOEVER, when the sediment was left to settle overnight, the acetone turned to a reddish colour. The supernatant acetone was removed, then the precipitated yellow fumarate harmaloid salts were washed with fresh acetone, just to observe that the fresh acetone also turned reddish!

It seemed somehow that acetone somehow converts the fumarate salts into an acetone-soluble reddish substance. This substance had a powdery substance when dry and did not dissolved in water.

go figure...

 

[69ron]

Sounds like harmala red forming.

This reminds me, when SWIM evaporates freebase bufotenine in acetone, it always forms a tiny bit of acetone insoluble material. It seems like acetone is causing some of the bufotenine to become bufotenine N-oxide.

It may be doing something like this to harmaline, causing it to oxidize into “harmala red”.

Is acetone known to cause oxidation?

 

[burnt]

Acetone can lead to artifact formation. N-oxides common artifcats from oxidative degradation.

http://www3.interscience.wiley.com/journal/113291779/abstract?CRETRY=1&SRETRY=0

here they report formation of artificats however base was also used in the extractions. But still acetone is reactive and doesn't surprise SWIM that some artifacts can form especially in normal atmosphere.