Harmala purification by solvents? Options
#1 Posted : 11/27/2020 7:43:56 PM

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Does anyone have practical experience and tips for purification of rue harmala bases or hydrochlorides using solvent extraction or recrystallization?
I've seen some threads here establishing some solubilities but I haven't found threads showing practical application.
Distillation is not a problem for me, but working with hot methanol would be. I wouldn't like to mix solvents that could not be subsequently separated. The relevant solvents I have in fair quantity are methanol, 95% ethanol, 91% isopropanol, 80% butanol, 98+% butanol if needed, acetone, butanone, and roughly 75% isopropanol 15% toluene 10% water. I have but don't expect to use toluene, xylene, and isoöctane as I'm trying to avoid azeotropes.

One thought was to simply dissolve the hydrochloride in hot ethanol or isopropanol, filter it, ice it, see how much crystal I get, then recover the rest by adding some water, distilling off the solvent, and manskeing the remainder.
Another idea was to try dissolving the freebase in methanol or hot ethanol, filter it, add 98+% butanol and cool it to get crystal. I'm working my way through 2,5 kilos of rue so if I had to fractionally distill a mixed solvent at the end it would be justified by the sheer quantity of harmalas.
But I have no feel for the solubility curves of these compounds in these solvents.

Good quality Syrian rue (Peganum harmala) for an incredible price!
#2 Posted : 11/27/2020 7:52:34 PM

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Just an idea, I do not have any experience:

What about to try something similar to mescaline re-x, which would mean to make sulphate salt of harmalas and let it crystalize from acetone/water?
#3 Posted : 11/27/2020 8:43:10 PM

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I have been considering experimenting with harmala sulfates. I doubt I would consume them as sulfates, since sulfates tend to give me more stomach issues than other salts. But your right, it could have potential as an intermediary in purification procedures.
Similarly, if I wanted to ensure poor solubility in butanol I could try the tartrates or malate. But I'm starting with the simplest.
#4 Posted : 11/29/2020 7:50:40 PM

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For its solubility properties as well as being monobasic, perchlorate would make a great anion - but you'd have to make absolutely sure no-one tried smoking the product!! Eating it probably wouldn't be so sensible either but again, it might well be a useful purification intermediate.
Ora, lege, lege, lege, relege et labora

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#5 Posted : 11/30/2020 6:16:33 AM

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Laughing I do have a quantity of perchlorate but I don't think I'll be going that route.
If I decide to get goofy it would be something others could safely replicate, like the ibuprofen salt.
Or perhaps a hydroethanolic recrystallization of monoharmaline glutamate Razz
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