THH 'Red'

[ijahdan]

Think I might have inadvertantly created a kind of 'Harmala Red' when drying out some thh I made by reducing harmaline. After reducing and precipitating with ammonia, I syphoned off most of the liquid and then poured the remainder along with thh into a pyrex dish which was the placed over a pan of water on a low boil. In the past Ive done this with a fan blowing across the dish and had no problems. This time I didnt use it and at some point in the process, the thh redissolved in the water, leaving a clear, deep red solution, in which state it remained on cooling.

I figure too much heat caused this but hope to salvage something by manske-ing and reprecipitating. Any input appreciated.

 

[Elrik]

So in essence, you had a mixture of THH freebase, ammonium acetate, ammonia, and zinc acetate.
My guess is applying heat drove off the ammonia, setting the THH into an equilibrium with the ammonium acetate with something like 1% of the THH being THH acetate at any given time [no need to do the math for real]. The continued heat drove the ammonia out of this equilibrium, letting more THH react with more ammonium acetate. And again and again until you had a beaker of THH acetate and zinc acetate.
I'd agree with your plan, add a squirt of vinegar to bring the pH <7 and manske it.
Alternately, if freebase is desired as the end product you should be able to just base it with room temp ammonia and this time filter the solids.

With the exception of the first one or two manskes when extracting seed, I've mostly only got trouble from working with harmalas in heated solutions.

 

[ijahdan]

Yeah it was all a bit rushed. Normally I wash the freebase several times before evaporating, which would have removed most of the zinc salts and ammonia acetates and prevented the formation of thh acetate. Hopefully I havent converted the thh back to harmaline. Ive never mansked thh before either and was planning to try your method of doing it at room temperature. Will report back with (hopefully successful) results.