• Members of the previous forum can retrieve their temporary password here, (login and check your PM).

Crystalline Caapi Alkaloids

Migrated topic.
I’m guessing that it’s all related to solubility. Harmala alkaloids are practically insoluble in water, so if only water is used, the alkaloids will precipitate out almost immediately, not allowing any time for crystals to form.

I think the alkaloids are very slightly soluble in alcohols, and this difference in solubility might slow the rate at which the alkaloids come out of solution just enough to form crystals.
 
acid was vinegar, base was lye

this was the same procedure I always follow for a/b on rue...only difference was I ran it on the filtered liquids instead of the harmala salts

mydriasis said he got the same xtals doing a STB on some rue, but that they lacked the structural integrity of gibran's once filtered.


I hope this isn't hijacking your thread gibran, if you'd like me to move it I will...I just figured since it was crystal harmala alks it fit here (although I just realized your thread specifically says caapi :oops: )
 
SnozzleBerry said:
...I hope this isn't hijacking your thread gibran, if you'd like me to move it I will...I just figured since it was crystal harmala alks it fit here (although I just realized your thread specifically says caapi :oops: )
It says caapi only because I used caapi alkaloids. (Actually, I didn’t want to experiment on my caapi alkaloids, so I used some of FV’s Caapi Copy, which I think is derived from rue). The crystallization should work regardless of the source of the alkaloids.
 
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.
 

Attachments

  • harmala1.jpg
    harmala1.jpg
    49.1 KB · Views: 0
elru said:
So you got harmala *salts* to form crystals in a mix (or kind-of mix) of acidic water & IPA? No base? What acid did you use?
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.
 
narmz said:
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?
 
gibran2 said:
Very nice! How did you get them? What was the process?

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.
 
narmz said:
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?
 
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.
 
Back
Top Bottom