starlight (Hive Bee)
01-11-03 12:39
No 397212
      best solvent for recrystallization of harmine?  Bookmark   

I have around 12g of Harmine/Harmaline hydrochlorides (impure from extraction). Any ideas on the best solvent for recrystallizing and the volume required?  methanol?

Just to clarify: the objective is not to separate the two alkaloids, simply to get rid of most of the other rubbish that may be in the powder i have.

01-13-03 20:43
No 397845
      modified from hasenfratz  Bookmark   

i got some very nice crystals (of mixed harmine/harmaline presumptive) by dissolving the mixed crude HCl salts (from the vinegar/salt method) in warm dH2O & adding ammonia water solution; after chilling, the mixed freebases precipitated out & were filtered & washed with icy water & then dried; the solid freebase powder was dissolved in enough warm 75% EtOH which was allowed to cool & evaporate a bit, thus reducing solution volume & ethanol percentage. a crystalline freebase (mixture of harmine & harmaline) resulted. the freebase can be used as is, or run through the manske/hasenfratz again(acetic acid & NaCl) for HCl salts...

don't you folks ever sleep?
(Hive Bee)
02-06-03 17:39
No 405125
      perhaps other bases?  Bookmark   

My SWF has also seen very decent reductions in volume between syrian rue and a manske extraction (not using vinegar at all). SWF thought that EtOH would get most of the NaCl, which she thought the major contaminant, but the results did not end up all pretty as expected, thus contaminants were suspected.

Converting to base form - could this be done via sodium bicarbonate or sodium hydroxide/potassium hydroxide? As for 'washing with cold water' would it really matter if the water was at 25-35 degrees C as is most tap water? I suspect that it might help to extract the bases into a non-polar solvent, DCM or naptha as you desire, as to ensuring no little bits got lost. Also even a filter would miss some of the base that comes out - a nonpolar, given time, would ensure that you missed none of it.

Would harm(al)ine freebase be more or less stable than the salt as regards to oxidation? Would a simple solution in - say - vodka - of this resultant freebase as resultant (mr gnrm23, where dost though getest thine ammonia from, those who make stinky-way wizzer would surely be curious) - pardon me, would it be possible to put the freebase into ordinary vodka type alcohol (whisky/gin/etc if you wish) and would this keep it longer (especially if stored in the freezer)?

questions questions, it is all I have isn't it...

I know naaaathing.
02-06-03 18:26
No 405147
      ammonia from the laundry section of local...  Bookmark   

ammonia from the laundry section of local supermaket (maybe hardware store of department store?) but make sure unscented & non-sudsing type only...
ya, other bases would prolly work as well... NaOH, or bicarb... but i was pretty much going by the book...
as for ethanol, i don't remember if it was 190 proof or 151 proof, but going from crude HCl salts to freebases & then back to HCl salts (using vinegar & NaCl again) gave a very pretty-looking end product...
now, what to do with too damned much MAOi harmalastuff... well, i hear it keeps pretty well, hehheh... maybe try & actually seperate the harmine from the harmaline? i dunno...

don't you folks ever sleep?