Harmala extraction - My quest for THH

[steppa]

Hey Nexus,

recently I began with my first harmala extraction with the ultimate goal of getting my hands on some THH in the very end.

Things are going pretty well so far. In the attatchment you'll find a pic of where I am now. The pic is taken after the first base percipitation after the first manske. Looking pretty good, eh?

I'll do another manske this evening. Do you guys think, when you look at the pic, that after another manske I could go to the harmine/harmaline separation step?

 

[steppa]

Ok. I did another manske, followed by another filtering and another manske. This evening I'll separate the harmine and the harmaline via selective percipitation with sodium bicarbonate and sodium carbonate. Then I'll move on to the zinc reduction. I hope to get there tomorrow.

 

[3rdI]

looking good steppa, i like doing rue extractions, basing out the alks and watching them swirl just before you reach a high enough Ph never fails to entertain me.

ive not done a THH reduction yet but i need to get on it this year, keep us informed on how it goes.

good luck

 

[steppa]

looking good steppa, i like doing rue extractions, basing out the alks and watching them swirl just before you reach a high enough Ph never fails to entertain me.

Yeah, this is the fun part. But I have to say that the initial filtering runs were a major pain in the...uhm...butt. I'm glad my vacuum pump didn't melt. *g*

keep us informed on how it goes.

Will do. I think I'll post another pic or two this evening or tomorrow morning.

 

[3rdI]

filtering rue is a nightmare, i do it through a t-shirt in a funnel, I must get a vacuum filter set up.

 

[endlessness]

Steppa, remember to do the separation twice, so do a first separation, and redissolve your harmaline part and re-separate it with sodium bicarb to get rid of most of the contaminating harmine. Hopefully your rue has good amounts of harmaline, I've had some that had a lot, and some that were mostly harmine.

How are you planning on separating the zinc from the THH?

And yeah filtering rue has it's tricks. Doing a propper manske with slow crystallization helps, and so does filtering repeatedly with progressively tighter cotton plug before precipitations. Also you can use multiple funnels at first.

Vacuum filtering is also def a great thing, and if you can't afford an electric pump, you can get a hand pump like mityvac silverline, it works really good.

 

[steppa]

Steppa, remember to do the separation twice, so do a first separation, and redissolve your harmaline part and re-separate it with sodium bicarb to get rid of most of the contaminating harmine.

That was my plan. I did some homework after we talked in the chat the last time.

Hopefully your rue has good amounts of harmaline, I've had some that had a lot, and some that were mostly harmine.

We'll see. But I noticed different colors when holding my used vessels under UV light. Greenish/yellowish (Harmine?) and blueish (Harmaline?)

How are you planning on separating the zinc from the THH?

From what I read it's as easy as dissolving the THH in 99% IPA which would/should leave the zinc behind and then decanting the solution. What do you think about this?

If this isn't supposed to work I'd have to draw on nexus's expertise.

Another thing I'm unsure about is the ammount of zinc to be used. Any tipps on this?

 

[steppa]

Due to a little ...mistake... I wasn't able to do the harmine/harmaline separation yesterday and the alkaloids had to undergo another base precipitation and an additional manske. Hopefully I'll get it done today.

But at least, they look much more pure now.

Have some pics of the precipitated alkaloids...

 

[smokerx]

Looks beautiful :thumb_up:

 

[Jees]

What is the plan to go forward with, once you get THH please?

 

[steppa]

What is the plan to go forward with, once you get THH please?

Sampling it. Seeing what it does.

 

[steppa]

so...I am done. Sort of I guess. I did the separation, I did the reduction. I decanted and filtered the result..then added basic solution and filtered off the result. I did dissolve the result in 99% IPA. Something that is supposed to be zinc oxyde did not dissolve and was filtered off. The IPA was evapped and something that it supposed to ba a powder that contains THH was aquired. Main quest completed. On this quest I earned some skill points +50 XP on patience and +20 XP on overall chemistry knowledge.

On a side note: I am glowing, everything is glowing under UV light here. Even my wife glows in her face and on her hands although she had nothing to do with the extraction.

My overall yields were bad. It yielded me 0.736g Harmine and 0.294g "supposed to contain THH powder".

I attatched one picture of the harmine, and one with a comparison of store bought harmine freebase, selfmade harmine freebase and my end result (left to right).

I am not sure about how well the reduction turned out. At least an UV light comparison shows differences to the colors of the harmine as well as to harmaline This is why I suppose it might have worked (at least to a part).

I think I will sample some of it and probably use the rest for changa. We will see.

 

[DreaMTripper]

Interesting result steppa, what was the starting amount of harmine? Will be interested to read what effects it gives!

 

[tregar]

Great work Steppa!

 

[steppa]

Interesting result steppa, what was the starting amount of harmine? Will be interested to read what effects it gives!

As I started with seeds I do not know the starting ammount. But I am sure I lost much product along the way due to some errors I made. To be honest, I hoped for a much better yield. But then again, this was not about getting the harmine.

@Tregar

Cool to hear that from you, as your experiments were the reason for me to start this operation. Thank you.

 

[endlessness]

How much harmaline did you begin with before reduction?

Hopefully it worked out. Let's get that tested in some manner or other. Do you have some ehrlich or can you buy some online (check colorimetrics thread in my signature link)? According to trout's notes, THH should turn blue with ehrlich after 24 hours (slow reaction), while harmaline should not.

 

[steppa]

How much harmaline did you begin with before reduction?

I did not let it fully dry to weight it.

Hopefully it worked out. Let's get that tested in some manner or other. Do you have some ehrlich or can you buy some online (check colorimetrics thread in my signature link)? According to trout's notes, THH should turn blue with ehrlich after 24 hours (slow reaction), while harmaline should not.

If the reduction somehow did not fully work out. Could one separate harmaline from thh?

Edit: Will have some marquis reagent next week...if this could be of help.

 

[Auxin]

The current consensus seems to be that THH is not crystallized out via the manske method, so the THH freebase could be precipitated from a filtered and basified manske.

 

[steppa]

The current consensus seems to be that THH is not crystallized out via the manske method, so the THH freebase could be precipitated from a filtered and basified manske.

Ok. I did this.

I took the 294mg harmalin/thh powder and did a manske on it. The manske yielded 146mg pretty pure looking harmaline HCL needles (Pics attatched). The following basification and filtering yielded 46mg retrievable powder (supposed to be THH then?). I couldn't get the rest out of the filter. I guesstimate another 30mg or so beeing stuck in the filter.

Later the day I will possibly post a picture of a comparison under UV-Light.

 

[steppa]

Ok. I think this didn't work out as it was supposed to.

I took the round about 300mg of the "supposed to contain thh" powder and did a manske on it to separate possible harmaline from possible thh. After manske and filtering I had 146mg of what I think to be Harmaline HCL. Then I based the solution with NaHO and filtered. I got 46mg of what I thought to be thh (+ another 30mg or so which are stuck in the filter). Then I did a black light test. From my understanding there should be a visible difference between Harmaline and THH...but...look what I've got. (left to right Harmine, Harmaline,..uhm..Harmaline?)