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Pure Extraction of Harmala Alks From P. Harmala Options
 
drellahcl
#1 Posted : 3/23/2009 6:25:39 AM

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Drella Syrian Rue Extraction

Harmine Extraction -

1. Mix Powderized seeds with very dilute sulphuric acid and add salt to the liquors.
2. Mixed alk hydrochlorides will be precipitated within 1-3 hours.
3. Redisolve hydrochlorides in water and warm to 50 Degrees and decolorise with Ammonia.
4. Purify Harmine by crystallisation from methyl alchohol containing benzene.

Harmine will appear white/colorless.

Conversion:

Reduce harmine with sodium in amyl alch to yield tetrahydroharmine.

-
This extraction can also be used on p. incarnata/caapi.

For highest yields Syrian Rue should be used. they contain about 4% harmala alks, harmaline is about 2/3 of it.

Any questions please ask.
- drella.
"I tried making sense of it, and then I realized I should be trying to make sense as to why I was even trying to make sense... "
 

STS is a community for people interested in growing, preserving and researching botanical species, particularly those with remarkable therapeutic and/or psychoactive properties.
 
endlessness
#2 Posted : 3/23/2009 9:46:52 AM

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drellahcl wrote:
Drella Syrian Rue Extraction

Harmine Extraction -

1. Mix Powderized seeds with very dilute sulphuric acid and add salt to the liquors.
2. Mixed alk hydrochlorides will be precipitated within 1-3 hours.
3. Redisolve hydrochlorides in water and warm to 50 Degrees and decolorise with Ammonia.
4. Purify Harmine by crystallisation from methyl alchohol containing benzene.

Harmine will appear white/colorless.

Conversion:

Reduce harmine with sodium in amyl alch to yield tetrahydroharmine.

-
This extraction can also be used on p. incarnata/caapi.

For highest yields Syrian Rue should be used. they contain about 4% harmala alks, harmaline is about 2/3 of it.

Any questions please ask.
- drella.



thanks for this tek

there are a few possible issues some people might find, though.. many people here have been doing food safe harmala extractions using vinegar in the first step, pure salt, and sodium carbonate in the basing step. So using sulfuric acid and the methyl/benzene solvent might be a disadvantage..

Also, the way to purify in other teks has usually been to repeat the whole process.. A few teks using some kind of solvent to redissolve the alkaloids have been proposed but there were issues with it

you say use methyl alcohol with benzene. Benzene is a known carcinogen, and methy alcohol is also toxic, so if using that in the last step one should be VERY careful there are no traces of these when evaporating.

Is the benzene really necessary?

Another thing, it seems that when evaporating harmalas in any kind of alcohol or acetone, some of the harmaline into a red goo called 'harmala red' or 'turkey red', which might be an n-oxide or something else, and the activity of which is still unknonwn. Did you never had this issue? Maybe the benzene has something to do with this, but is it worth it?

you mentioned 4% yields with rue, even after purification? how clean are the crystals?

and lastly, you mentioned this can be made with p. incarnata. Any idea what kind of yields one can get with that?

thanks Smile

 
Phlux-
#3 Posted : 3/23/2009 9:52:25 AM

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drellahcl
#4 Posted : 3/23/2009 11:39:20 PM

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hello endlessness,

If sulfuric acid is an issue for step 1 vinegar/lemon juice, can be used as well as food safe alternatives.

Using iso, acetone, or Etoh will yield this "harmala red". I have never had this problem using methyl alchohol with benzene. 1:1

Harmine had a mp of 255-257 which indicates there should also be no problem with trace amounts left behind with extracted harmine.

Methyl/Benzene are toxic, however with proper ventilation they can be safely used.

I have crystallized harmalol from p. harmala using only methyl.
So this route might be just as effective for Harmine.

P. Incarnata yields have varied from specimen to specimen. .5 to about 2% Mature plants having higher alk.

Any other questions please ask.

- drella.















"I tried making sense of it, and then I realized I should be trying to make sense as to why I was even trying to make sense... "
 
endlessness
#5 Posted : 3/23/2009 11:45:59 PM

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very nice info, thanks a lot!

maybe some mix of ethyl and limonene could substitute the methyl/benzene and not form harmala red... would be interesting to find this out


SWIM has P.Incarnata growing, it is a few years old already.. what is the best way of using that? Just normal drying the leaves first and grinding them and then proceeding to the extraction?

welcome to the forum, btw
 
drellahcl
#6 Posted : 3/26/2009 11:21:08 PM

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Glad to lend some help : ]
And thank you,

Substituting with ethyl and limonene would be interesting to try, That will have to be a project in the near future.

Normal drying the leaves/then to extraction works great. I normally dry the leaves at room temp and store until needed.

Also an advantage to growing the plant is having access to the fruit. There is usually 0.25% alkaloids in fruit rinds.



"I tried making sense of it, and then I realized I should be trying to make sense as to why I was even trying to make sense... "
 
kemist
#7 Posted : 5/22/2009 8:30:47 PM

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Sorry but this tek is rubbish. ILPT would never commit to proceed seeds like that. He didn`t mention filtering or decantation after first step! For newbie it can cause catastrophe as after literally following this tek he end up with seeds mush and harmala hydrochlorides in one containerCrying or very sad
And how about those fancy chemicals methylbenzene or sulfuric acid ? Shocked


All what one need is vinegar, rock salt, bicarbonate soda(heating 2-3 hours at 200C will convert into Sodium carbonate Na2CO3 ) and distilled water.

ILPT experienced rock salt(Tesco`s own brand,89pence for 500grams ) to be fairly dirty Shocked (even it`s food grade )

He recommended to recrystalize salt from distilled water. For first salting one can use that dirty rock salt but for second salting(it`s actually cleaning of product)pure salt should be used

As a kemist I never met ILPT in physical form and never talk to him. He share his wisdom, trough my mind, telepathicly only. Please don`t prosecute me, for his possible illegal activities. He is bonkers about chemistry and doesn`t even exist in this primitive reality !!!
 
soulfood
#8 Posted : 5/23/2009 12:58:07 AM

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I've noticed some greyish black particles settle in the heating vessel when using some rock salt. I just pour the liquid off leaving these visible impurities behind.

Are you saying that there are soluble impurities also?
 
kemist
#9 Posted : 5/25/2009 7:58:27 AM

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soulfood wrote:
I've noticed some greyish black particles settle in the heating vessel when using some rock salt. I just pour the liquid off leaving these visible impurities behind.

Are you saying that there are soluble impurities also?


Well not really....
ILPT decanted as you did,left some shit behind.After that he ran decanted salt solution trough the funnel with compressed cotton . ILPT ran trough this cotton about 700 grams of rock salt in 2,2 l of distilled water and it took 5-6 hours. He wanted concentrate it really tough and let crystalize but he accidentally boiled off all water and and up with finer white powder. Salt is white clean and lost that hint of sulfuric smell and taste.

... Anyway check out the residue after filtration
As a kemist I never met ILPT in physical form and never talk to him. He share his wisdom, trough my mind, telepathicly only. Please don`t prosecute me, for his possible illegal activities. He is bonkers about chemistry and doesn`t even exist in this primitive reality !!!
 
tryptographer
#10 Posted : 5/30/2009 7:59:45 PM

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Why not use common table salt? It's highly purified. Traces of iodine won't hurt.

I'm always interested in alternative teks so thanks for posting - although I'll avoid benzene like the plague Pleased

Quote:
Conversion:
Reduce harmine with sodium in amyl alch to yield tetrahydroharmine.


That's interesting! THH is hard to get here, and separation from other harmalas is probably too difficult. Unfortunately, few people will have metallic sodium... any strong reductors that can replace the sodium? I'm thinking about magnesium, aluminium, zinc powder in dilute HCl...

And why in amyl alcohol - to moderate the reaction? Incredibly foul smelling stuff.
 
kemist
#11 Posted : 5/30/2009 8:29:30 PM

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tryptographer wrote:
Why not use common table salt? It's highly purified. Traces of iodine won't hurt.

I'm always interested in alternative teks so thanks for posting - although I'll avoid benzene like the plague Pleased

Quote:
Conversion:
Reduce harmine with sodium in amyl alch to yield tetrahydroharmine.


That's interesting! THH is hard to get here, and separation from other harmalas is probably too difficult. Unfortunately, few people will have metallic sodium... any strong reductors that can replace the sodium? I'm thinking about magnesium, aluminium, zinc powder in dilute HCl...

And why in amyl alcohol - to moderate the reaction? Incredibly foul smelling stuff.


Any impurities can cause side reaction and byproducts, one never know.ILPT prefer to have evrything crystal clean(as far as kitchen can get) Cleaning NaCl via Crystalization is the simpliest thing ever. But each their own, lazy bums can use table salt or uncleaned rock salt it`s their business ILPT just wanna share what he found

Yeah you can use lithium and 10 % solution of isopropylalcohol (IPA) in anhydrous ammonia Shocked

If you look on this table of reducing agents that`s such a sorrow Crying or very sad

....other method is using Platinum and Palladium catalysators with hydrogen at high pressure, so one definitely need autoclave Shocked Shocked Shocked

There is no chance for KEMIST to do that in kitchen!!! That`s serious job for chemists, sorry Sad
As a kemist I never met ILPT in physical form and never talk to him. He share his wisdom, trough my mind, telepathicly only. Please don`t prosecute me, for his possible illegal activities. He is bonkers about chemistry and doesn`t even exist in this primitive reality !!!
 
tryptographer
#12 Posted : 5/30/2009 10:02:32 PM

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I'll be a lazy bum and leave the purification to the salt companies Pleased

I just found out the manufacturers add some ferri- and ferrocyanide to table salt as anti-clumping agents, and sometimes of course iodide (like 50 mg/kg or less). Iodine-free salt is sold too, no problem. I'm even thinking of trying calcium chloride instead, much higher solubility than NaCl.
That pound of beautiful Rue seeds is waiting...
Quote:
If you look on this table of reducing agents that`s such a sorrow Crying or very sad

Ouch, nice tip, thanks. So, I guess the harmala reduction belongs in the aromatic ring column. Not like the reduction of DMT-n-oxide at all. A waste of time to try this in the kitchen indeed... thanks for sharing!
 
kemist
#13 Posted : 5/31/2009 9:04:30 AM

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tryptographer wrote:
I'll be a lazy bum and leave the purification to the salt companies Pleased

I just found out the manufacturers add some ferri- and ferrocyanide to table salt as anti-clumping agents, and sometimes of course iodide (like 50 mg/kg or less). Iodine-free salt is sold too, no problem. I'm even thinking of trying calcium chloride instead, much higher solubility than NaCl.
That pound of beautiful Rue seeds is waiting...
Quote:
If you look on this table of reducing agents that`s such a sorrow Crying or very sad

Ouch, nice tip, thanks. So, I guess the harmala reduction belongs in the aromatic ring column. Not like the reduction of DMT-n-oxide at all. A waste of time to try this in the kitchen indeed... thanks for sharing!

Well one didn`t mention biochemistry. They are some enzymes which can do job peacefully whilst chemists have to use violence (high pressure, temperatures or aggressive chemicals). Sorry but I don`t know much about biochemistry....

Is not impossible you know, actually is very enjoyable. Only preparation of anhydrous ammonia is exciting task....
and SODIUM METAL is beauty itself.... remember how me and mate were literally chopping Shocked (with hammer and axe Shocked ) 50 kilos Shocked of Na at work. It took us whole shift to made smaller portions of it..... lovely times..... really missed that crazy company i worked for...
As a kemist I never met ILPT in physical form and never talk to him. He share his wisdom, trough my mind, telepathicly only. Please don`t prosecute me, for his possible illegal activities. He is bonkers about chemistry and doesn`t even exist in this primitive reality !!!
 
 
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