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Theoretical tek to simplify seperation of harmine/thh from hcl/zinc reduction Options
 
The Day Tripper
#1 Posted : 4/25/2012 6:10:32 AM

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Reading this thread on freebasing the salt water after a manske, to get the other beta-carboline hcl alkaloids that won't precipitate, gave me an idea.

I wonder if this method could be used to separate thh from harmaline/harmine, since I've heard thh hcl won't precipitate out when manske'd.

Can anyone confirm that thh hcl won't precipitate in a manske?

I've heard it mentioned before, but can't be sure.

This would be especially useful if you were to do a zinc/hcl reduction of already manske'd rue hcl alkaloids (so theres no other alkaloids that will precipitate out when freebased), but not separating the harmine/harmaline via the baking soda/washing soda method first. As well, its been shown that its rather difficult to separate the harmine/harmaline via baking soda/washing soda method and get pure(ish) harmine and harmaline separate without doing repeating the process several times.

The harmine/harmaline hcl would precipitate out (most of it at least) when manske'd, and assuming your reduction worked, and the harmaline was reduced to thh, it would be mostly harmine hcl since the zinc/hcl won't reduce the harmine.

Basify the manske water, then filter and collect the zinc contaminated thh freebase.

Then per shulgin's method of recrystallizing thh in the thikal entry, dissolve it in minimal dry warm ipa, filter out any zinc that would not be soluble in the ipa, then add a guesstimated amount of %30 hcl dropwise, cool, and filter/wash with cold dry ipa to get thh hcl xtyals.

No need for ammonium chloride to prevent the zinc from precipitating, since its not soluble in the ipa in the first place.

Seems like an easier way to do the zinc/hcl reduction, without having to separate the harmine/harmaline first, as it won't reduce the harmine anyway, and thh won't manske out.

The dry alcohol recrystallization of the thh would ensure no extra zinc/aluminum/whatever metal you used for reduction, ends up in your thh end product, as would happen if you just naoh/koh freebased it out after the manske, and redissolved in dilute hcl and evaporated.

To summarize-

Take pre-manske'd rue hcl's, preform a zinc/hcl reduction, another manske to get harmine hcl, freebase, collect thh fb w/ zinc/aluminum contaminants, dissolve in dry warm ipa, filter out any zinc/metals, then add concentrated hcl to precipitate thh hcl, and finally wash with dry cold ipa.

Alternatively you could start with pure harmaline, but i see it as unnecessary assuming the reduction step converts most of it to thh.

Any thoughts or suggestions on this idea?

Thanks-
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