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DHH->THH reduction results I can't make sense of Options
 
Jagube
#1 Posted : 12/10/2019 1:42:40 PM
I performed a zinc reduction on a mix of harmine and harmaline, obtained by manske.

Normally I separate them, but this time I didn't.

The solution glowed green in UV initially, and lost its glow after the reduction.
I crashed it out, filtered, washed with ammonia water and dried in a heated propagator. I also blew a fan over it, but for a short time, maybe an hour, before I realized it's better not to use air drying to prevent oxidation and put it in the propagator.

The result seems to be harmine and harmaline, as it doesn't feel like there is THH in it and the effects of 400mg of it are very strong. If it was THH, that would be roughly 200mg harmine and 200mg THH, which I've taken many times before and was nothing like this. Also there is no THH feel and there is a harmaline feel.

When I redissolved this in order to separate the two alks, it glowed green, but mildly.
The first fraction crashed out at pH 7.3 going down to 6.5, the second fraction crashed out at 9.3 going into the 8's.

Now, I'm wondering if my reduction wasn't complete or the THH converted back to harmaline during the drying process?
 
blue.magic
#2 Posted : 12/12/2019 11:04:46 AM
I doubt your THH would oxidize back that easily. I have dried the freebase with heat and air without any problems. A tiny bit still made a vinegar glow blue strongly.

What was the concentration of the reaction mixture?

Perhaps your two alkaloids rapidly co-precipitated and your THH got crubled with harmine so it hindered it.

I would suggest redissolving everything to 10 g/L concentration, then very slowly pH-separate with 5% ammonia.
 
 
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