Somewhat related info here: I took some freebase harmalas and dissolved them in a minimal amount of acidic water. SWIM slowly layered 2-3 times the amount of IPA using a syringe on top of the water layer. Minimal whispy clouding formed at the interface between the two layers, and let this set for 2-3 days. Came back to it and the clouds had gone, but down towards the bottom of the glass spherical hedgehog shaped crystal formations have begun to inhabit the glass. UV light shows there is still harmalas present in solution, and the coloration of the liquid from top to bottom shows that there is still more alcohol on top and that both layers have not yet fully mixed. SWIM is thinking this is taking a long time because of the difference in density between water and alcohol, with alcohol being less dense and being on top, it takes a long time to fully mix. So maybe if the water was layered carefully on top of the alcohol, the mixing process would take much less time.

This works because most salt-forms of harmalas are moderately insoluble in IPA, though a small amount can dissolve(prolly more so in ethanol as it is more polar than IPA), and as the ratio of alcohol to water slowly changes and becomes more alcoholic, the harmalas very slowly precipitate out. The crystals appear to be very strong, they are very white and transparent looking with spikey shards pointing out from the circular formation sites.

I think with layering your liquids you can achieve very high purity if you are patient. You can easily use this same method to layer your basified water on top of your harmala saturated water to get freebase. Syringe is best for this, but anything long you can lay at an angle and pour the liquid down, like a butter knife, works to prevent it form splashing in and dropping instantly and mixing quickly.

Harmala salts in crystal form are easy to come by. In fact, a Manske produces really beautiful hydrochloride salts (see attachment). Getting harmala freebase to crystallize seems to be much more rare, hence this thread.

@ narmz – It would be nice if you could post a photo of your crystals. Interesting.

Yep, I believe I used citric acid with this one, I've been experimenting with fumarates and citrates.

Gibran2 - I was mostly giving an example of a way to slow-grow crystals of high purity. Regardless of whether it's a freebase or salt form, slow growing crystals will result in higher purity, and you can always jump between the two to end up with what you want. Just figured it was related cause we're talking about using alcohol for crystallization.

I'll post some pictures once it's finished precipitating and I've dried them, they look like little white orbs right now, just got a fancy camera so I'll get to take some up-close pictures and get all nerdy wit it.

As far as I can tell, crystalline freebase can easily be achieved without alcohol simply by introducing the basic solution to the alkaloid solution at a slow rate.

Any photos?

Very nice! How did you get them? What was the process?

omg beautiful!!

This is the results of your caapi tek. The second freebase step, 4grams of lye dissolved in 30-40ml of water, slowly added drop-wise to the harmala acetate solution. Thanks for the tek BTW! Still gotta decant and run water through them a few times, but they are looking very nice.

Did you stir as you were adding the base?

Nope, just slowly added, looked like whispy clouds at first. Over the course of the next few hours crystals formed.

Interesting, I'm going to try this out.

Oh god, look at those crystals narmz! A simple, slow dropwise introduction of basic water produced that?

I have been stirring like crazy while I added the base, but I think I need to reevaluate my procedure...

Great, I going to experiment on making crystals from (rue) harmalas.

I want to try to crystalize them from acided solution with just noah like namz.

Namz can you tell me something about amounts.

How much ml vinigar should I use for one gram of harmalas.
How much basified solution should I drop in ?

Thanks

ok I tried it, it didn't really work for me because I was going to fast at first. I ended up getting some crystals when I slowed down. I used a basic solution 5g/lye in 50ml of water. A good speed seems to be about 2-3 drops per minute no faster. keep adding the base until you don't see precipitation any more. I think it will work much better next time I try now that I know what rate to use

Hey guys it has been awhile. Great looking work. I was looking for the acetone harmala info in wiki, couldnt find it anyone hook me up with a link? Also, any developments with the harmala fumeric salts? I am moving in more of a pharma direction and would really like to perfect the salt side harmala. Keep up the great work. Peace.

Im not sure fiorsir, maybe harmalas being very poorly soluble in acetone has something to do.. Though I never tried making fumarates from harmalas.

I am conducting an experiment as we speak, but with water, fumaric, and harmala freebase. I will post the results.

Looks like I got something going here.
These are not caapi but rue crystals.

I have spend 30 minutes adding small drops

Incredible!

Let us know if they stay that white after drying!