Harmine, harmaline and THH from Syrian Rue. Verification and finetuning of the VDS-protocols

[Orion]

The trouble here is that magnesium hydroxide or its carbonate will be as insoluble as freebase harmalas, and will also dissolve in the same acids as harmalas. I'm not sure what other folks did when using magnesium ribbon, but I took advantage of the fact that magnesium ammonium phosphate (MAP) is highly insoluble. By using phosphoric acid along with the magnesium ribbon, it was then possible to precipitate the MAP by careful addition of ammonia. The MAP crashes out as a dense, pure white powder at a pH sufficiently distinct from either harmine or harmaline that these compounds are very easy to tell apart from the MAP. I (or maybe @downwardsfromzero) documented the pH measurements somewhere around here a couple of years or so ago.

I get blobs of something when adding ammonia the first time. It happens at pH levels too low to be harmalas, the same as seen in the video in Q21Q21's post above. I assume this is some kind of magnesium salt? I could probably remove at least the visible stuff by filtering this off before going high with the pH. I have a slight concern that it may have an effect like I described at the end of the first post in this thread regarding excess sodium bicarbonate trapping alkaloids: Rue to separated freebases with less fuss.

After doing a manske on the entire precipitate and then basing again, there was nothing strange about the precipitation and I was able to get different fractions out with a clear pH gap between.

So I'm wondering, do I do the same thing again with this higher pH crashed portion of it, or go straight to manske? I'm feeling like a manske makes more sense, that way the one and only basing should be cleaner as the magnesium salts will already be disposed of.

As for the phosphoric acid approach, I could try that on another batch. It does seem like a manske takes care of the strange globs but one less step would be nice.

 

[Transform]

I get blobs of something when adding ammonia the first time. It happens at pH levels too low to be harmalas, the same as seen in the video in Q21Q21's post above. I assume this is some kind of magnesium salt? I could probably remove at least the visible stuff by filtering this off before going high with the pH. I have a slight concern that it may have an effect like I described at the end of the first post in this thread regarding excess sodium bicarbonate trapping alkaloids: Rue to separated freebases with less fuss.

After doing a manske on the entire precipitate and then basing again, there was nothing strange about the precipitation and I was able to get different fractions out with a clear pH gap between.

So I'm wondering, do I do the same thing again with this higher pH crashed portion of it, or go straight to manske? I'm feeling like a manske makes more sense, that way the one and only basing should be cleaner as the magnesium salts will already be disposed of.

As for the phosphoric acid approach, I could try that on another batch. It does seem like a manske takes care of the strange globs but one less step would be nice.

Sounds like the globs were most likely magnesium hydroxide, if they formed around the drops of ammonia. Were you able to observe closely how the precipitate formed?

I'd be inclined to agree that going straight to a Manske after the Mg reduction would appear to make sense. I've seen contradictory reports on whether Manske works for THH or not, however. I've not tried it, since the MAP approach provided freebase rather easily - can anyone else comment on practical results of attempting Manske on THH?

 

[Orion]

Sounds like the globs were most likely magnesium hydroxide, if they formed around the drops of ammonia. Were you able to observe closely how the precipitate formed?

I'd be inclined to agree that going straight to a Manske after the Mg reduction would appear to make sense. I've seen contradictory reports on whether Manske works for THH or not, however. I've not tried it, since the MAP approach provided freebase rather easily - can anyone else comment on practical results of attempting Manske on THH?

I'll probably do that. I might try to reduce it a bit more by adding more vinegar and magnesium, chopped into the smallest pieces I can before spinning it at high speed. The reason being I expect to see some color difference by now under UV, since this was the redissolved product which only precipitated at a pH above 9.5. Hopefully after freebasing and rinsing with basic distilled water again I can actually see a difference this time.

I assume the bubbling is just hydrogen gas and isn't a crucial component of the reduction, correct?

As for the blobs, they form exactly like they do in the video in Q21Q21's post. As soon as the ammonia drop hits the solution, a white substance forms around it and stays there, spinning around in the solution before it has began to cloud up at higher pH when the actual harmalas crash.

 

[Flufferus]

this is a cool thread. i would be so hype if i could make clear harmala crystals like that!!