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Harmaline/harmine to THH - safe kitchen conversion tek required. Again. Options
 
Phlux-
#1 Posted : 11/23/2009 3:30:08 PM

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THH seems preddy costly - well at least compared to the price of rue.
Rue has plenty harmine and harmaline and it seems silly to not convert between them(reduction/oxidization)
Mercury amalgam is required to convert to thh but thats dangerous and not suitable for kitchen work.
What other reduction agents can be used ? - maybe that zink tek must be revisited.
Surely there is a lot of interest in this and enough ppl with skills for us to get together and make a nice tek. :Þ
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geeg30
#2 Posted : 11/24/2009 12:39:17 AM

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I read somewhere that Sodium Borohydride was successfully used to convert Harmaline/Harmine to THH. Its quite hard to find but is used in making certain Hydrogen fuel cells. There was a company in the UK selling 10g for £6 but they seem to have vanished or if you have a friend who can buy from sigma aldrich they also sell it. Used in small quantities it is semi safe but it is quite toxic and hazardous.
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Jorkest
#3 Posted : 11/24/2009 1:15:19 AM

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well FV can make or extract THH using food grade materials...well then SO CAN WE!
it's a sound
 
soulfood
#4 Posted : 11/24/2009 1:41:57 AM

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what about this (don't know where it's originally from):

Procedure: (Example) 10 grams of harmaline dissolved in 10% aqueous hydrochloric acid had zinc dust added gradually (with occasional shaking). The mixture was heated on a water bath until the yellow coloration disappeared. After filtering off any unreacted zinc, ammonium chloride was added to prevent precipitation of zinc hydroxide. Addition of ammonia caused an immediate precipitation of white material. This was shaken into Ethyl acetate; which recovered THH. (See Siddiqui et al. 1983 for their version of this procedure.) (This should also work for harmine) Siddiqui et al. 1983 reported that the addition of NH4Cl prior to basification with Ammonia increased the yield for this reaction from 50% to around 80% (by preventing the precipitation of Zinc hydroxide).

I'm not a chemist, but it seems kind of straight forward if you can think of a good substitute for ethyl acetate.
 
Observant
#5 Posted : 11/24/2009 1:44:24 AM

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Yeah - I still think its possible they extract from caapi leaves or another thh rich plant source .
Had he more quickly realized just who they were,he would have shown them more respect.Had he tried harder to fathom their brilliant minds,he would have taken more of their teachings to heart.Had he more clearly understood the purpose of their being,
he would have more vigorously tried to assist them.They were truly honorable; he was sadly prejudiced.
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soulfood
#6 Posted : 11/24/2009 2:00:39 AM

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Well there are some strains of caapi that are meant to contain mostly large amounts of THH and little else, but good luck to us all in finding them.

Turns out to make Ethyl Acetate from Ethanol:

In a test tube, mix 3 mL ethanol with 2 g sodium bisulfate and 3 mL white vinegar. Heat it gently. Sniff carefully. The sour smell of vinegar has turned into the fruity smell of ethyl acetate (CH3COOC2H5). It is a much-used solvent.

Well I've stumbled on a way of making sodium bisulfate, but now that's just getting even more complex... I'll post it anyway:

Sodium bisulfate is produced by two methods. One method involves mixing stoichiometric quantities of sodium hydroxide and sulfuric acid which react to form sodium bisulfate and water.

NaOH + H2SO4 → NaHSO4 + H2O

A second production method involves reacting sodium chloride (salt) and sulfuric acid at elevated temperatures to produce sodium bisulfate and hydrogen chloride gas.

NaCl + H2SO4 → NaHSO4 + HCl

The liquid sodium bisulfate is sprayed and cooled so that it forms a solid bead. The hydrogen chloride gas is dissolved in water to produce hydrochloric acid as a useful coproduct of the reaction.


hmm... maybe ethyl acetate can be switched to acetone? I don't know... I'v never even managed to come across ethyl acetate.

Apologies if this is crossing the line on board rules... I know talk of synthesis isn't allowed, but is that only for illegal substances, or is it synthesis in general?
 
soulfood
#7 Posted : 11/24/2009 1:15:30 PM

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Does anyone know the purpose of the amalgam in that proedure?
 
Observant
#8 Posted : 11/24/2009 2:34:12 PM

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soulfood wrote:
I don't know... I'v never even managed to come across ethyl acetate.


http://kremer-pigmente.d...030103&product=70300 (for Europe )
Had he more quickly realized just who they were,he would have shown them more respect.Had he tried harder to fathom their brilliant minds,he would have taken more of their teachings to heart.Had he more clearly understood the purpose of their being,
he would have more vigorously tried to assist them.They were truly honorable; he was sadly prejudiced.
They were exceedingly well informed; he was grossly ignorant.They were totally indefatigable; he so often, and so quickly,gave up. Still, for many years there was a strong inter-species alliance between the Eleven-Eleven of the Half-way Realm, their Seraphic Associates,and their flesh-and-blood friend, a common mortal. Much was accomplished, many profited, and, there’s only one regret...They could have achieved so much more...

All Hypnotizing Hypnotizes Hypnotizing
 
soulfood
#9 Posted : 11/24/2009 3:13:31 PM

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Oh sweet!

You know what? I actually love you Smile It's expensive to ship to me as I've used them for limonene, but this could be valuable to my bufotenine experiments also Smile
 
Infundibulum
#10 Posted : 11/24/2009 3:22:35 PM

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Guys, please try to tune a bit low. Synthesis discussions are not strictly allowed because of 2 main reasons:

1. They often require dangerous, nasty as well as watched chemicals. whoever mentions sodium borohydrate should be aware of this! Kitchen chemists and imaginary kitchen chemists have no reason to mess with stuff like this.

2. The procedures involved can be hazardous. Turning sodium bicarb to sodium carbonate is a totally benign procedure and fine, but making ether, ethyl acetate, refluxing etc are things that carry the risk of hazard!

what Phlux asked for was for a "THH - safe kitchen conversion tek", not a sodium borohydride reduction tek. There was a tek involving ascorbic acid, but SWIM thinks this is a highly unlikely tek to work. He doesn't know if any other tried it with success though!




Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
soulfood
#11 Posted : 11/24/2009 3:32:48 PM

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Infundibulum wrote:


what Phlux asked for was for a "THH - safe kitchen conversion tek", not a sodium borohydride reduction tek. There was a tek involving ascorbic acid, but SWIM thinks this is a highly unlikely tek to work. He doesn't know if any other tried it with success though!





Yeah, that didn't work. I gave that a very thorough try.

Obviously sodium borohydride is well out of the question and the notes I found on ethyl acetate were just for show, but discussing the use of ethyl acetate is ok right?
 
Infundibulum
#12 Posted : 11/24/2009 3:41:08 PM

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Aye, of course! Some people are able to buy ethyl acetate from where they live and it is also commonly used solvent in perfumes.

(and btw, I was re-reading the ascorbic acid conversion tek, the Nobuoni user does sound pretty dodgy and I am not sure if he ever really tried the tek or just theorising out of his ass)


Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
soulfood
#13 Posted : 11/24/2009 3:45:05 PM

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Yeah, he said he didn't try it himself. Either way I kept the reaction going for a good 8 hours and didn't even notice a hint of a change in colour and all the happened in the long run was I made my harmine get all sticky Smile
 
amor_fati
#14 Posted : 11/24/2009 3:52:46 PM

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Infundibulum wrote:
(and btw, I was re-reading the ascorbic acid conversion tek, the Nobuoni user does sound pretty dodgy and I am not sure if he ever really tried the tek or just theorising out of his ass)


That's what I was thinking as well. Sounded too good to be true.
 
soulfood
#15 Posted : 11/24/2009 11:41:51 PM

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So no one has any good/bad feelings on the process I quoted?
 
Infundibulum
#16 Posted : 11/25/2009 1:26:07 AM

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Quote:
Procedure: (Example) 10 grams of harmaline dissolved in 10% aqueous hydrochloric acid had zinc dust added gradually (with occasional shaking). The mixture was heated on a water bath until the yellow coloration disappeared. After filtering off any unreacted zinc, ammonium chloride was added to prevent precipitation of zinc hydroxide. Addition of ammonia caused an immediate precipitation of white material. This was shaken into Ethyl acetate; which recovered THH. (See Siddiqui et al. 1983 for their version of this procedure.) (This should also work for harmine) Siddiqui et al. 1983 reported that the addition of NH4Cl prior to basification with Ammonia increased the yield for this reaction from 50% to around 80% (by preventing the precipitation of Zinc hydroxide).

This one? This does sound pretty much fine, easy and it is also published. Note that you do not really need the ethyl acetate since THH precipitates out of the solution by itself. Ethyl acetate is used as the solvent to recover it and separate it the precipitate from any impurities.

If anyone tries it just make sure one has as pure harmine/harmaline as possible. If there are impurities you don't know what it may be reduced to. Remember the GIGO chemistry principle (Garbage In, Garbage Out)


Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
soulfood
#17 Posted : 11/25/2009 1:40:09 AM

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Well that's reassuring...

it's a shame I'm living with my folks for at least another 6 months though Sad
 
Phlux-
#18 Posted : 11/25/2009 8:06:16 AM

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hrmm - now to just find a local zink dust supplier.
antrocles wrote:
...purity of intent....purity of execution....purity of experience...

...unlike the "blind leading the blind". we are more akin to a group of blind-from-birth people who have all simultaneously been given the gift of sight but have no words or mental processing capabilites to work with this new "gift".

IT IS ONLY TO THE EXTENT THAT WE ARE WILLING TO EXPOSE OURSELVES OVER AND OVER AGAIN TO ANNIHILATION THAT WE DISCOVER THAT PART OF OURSELVES THAT IS INDESTRUCTIBLE.


Quote:
‹Jorkest› the wall is impenetrable as far as i can tell


Quote:
‹xtechre› cheese is great


He who packs ur capsules - controls your destiny.

 
Madcap
#19 Posted : 11/25/2009 11:26:19 PM

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I got zinc from a fireworks supply. Is this safe to use in this procedure? I'm wondering if the purity is up to the task...
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soulfood
#20 Posted : 12/11/2009 5:16:19 PM

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Has anyone tried this yet?

I guess you got to have some pretty damn clean xtals first.
 
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