How do you go from harmala HCl's to the acetates?

[Jagube]

The HCl's are a bugger to work with, because they're poorly soluble and whatever you want to do after Manske requires dissolved alks (filtering, ammonia-based separation, zinc reduction...).

In the extraction I'm currently doing, I couldn't dissolve my HCl's and keep them dissolved for long enough to be able to do anything with them. I found myself re-heating the mixture repeatedly as the HCl's would recrystallize promptly.

I decided to bring it to a high temperature, base with NaOH, collect the freebase and re-dissolve in vinegar. The reason I chose NaOH was the volume was already large and I didn't want to waste a lot of ammonia.

I followed through with the plan, but upon basing I realized the freebase was falling on a layer of HCl's!

I'm going to add vinegar to dissolve the freebase and hopefully after that there won't be a lot of HCl's, so I can repeat the heating / basing process with less headaches.

 

[blue.magic]

I do it like in VDS protocols, usually just prepare hot 3% acetic acid (basically hot vinegar) in which I dump the freebase harmalas. The I continue with filtering, separation etc.

Harmala hydrochlorides are freely soluble in hot water, but poorly soluble in cold. In cold water, you can get only 2.5% w/v solution.

I never had the problem so far, always using hot water for dissolving hydrochlorides (65 °C and hotter). I use thick walled beaker wrapped in alu foil.

I acutally have the opposite problem, solution cooling down too slowly so instead of nucleation and crystallization, I get supersaturated solution - a light scraping of the glass than causes sudden crashing of everything :d

I am now working on salt-free tek since it is very easy to convert base to HCl directly.