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THH extraction tek

Migrated topic.
I will definitely try this some day soon.

Btw, if I precipitate rue by increasing the pH, would there be many other alkaloids in it than harmine/harmaline?

Do I have to salt it out to get clean harmine/harmaline?
 
salting out removes vasicine and vasicinone from it, so its only harmine/harmaline basically, and some other plant impurities

but remember to get pure harmalas, you have to repeat the steps at least a couple of times. First time for SWIM comes out dark brown powder.. second time a nice light brown/pinkish powder.. SWIM didnt do more than this yet because he is happy with what he got for now, but for sure sometime he will do more consecutive repeats to get really pure stuff
 
Saturated salt solution in the fridge for a few days gives good yields from Rue'
Then salt it out again'
Dry the resultant goo' crush it up fine' and wash in warm methanol/ethanol'
The salt you used to push out the harmine hydrochlorides falls to the bottomof the flask'
the Harmine hcl dissolves in the warm alcohol'
Draw off the alcohol'
Evaporate on a plate'

Bliss'
Nobuoni +
 
Wow Nobuoni, thanks for the informative posts!

Let me be the first to Welcome you to the forum of nexus, your apparent knowledge of chemistry is a fresh sign of good things to come :)
 
Thank you for the warm welcome bro'

I updated my original post after a little bit more study' and hope that it answers some folks questions a bit clearer'




Hamine/Harmaline conversion to THH with food grade and H2O'


Harmine takes up four atoms of hydrogen when treated with sodium and alcohol' and is converted into tetrahydroharmine'

Hence the oxygen atom is knocked off and replaced by hydrogen' converting Harmine/Harmaline to THH'



Ascorbic acid (vitamin C)

Ascorbic acid (vitamin C) is a water-soluble, antioxidant present in citrus fruits, potatoes, tomatoes and green leafy vegetables.

One important property is its ability to act as a reducing agent (electron donor).
Ascorbic acid is a reducing agent with a hydrogen potential of +O.08V, making it capable of reducing such compounds as a molecular oxygen'

So simply put'
Add your Harmine/Harmaline to a strong solution of ascorbic acid and H2O' and heat gently' until the yellow colour has changed to a clear solution'
Of what happens is the ascorbic acid attracts the oxygen and the production of H2O2 donates a hydrogen'
Hydrogen peroxide H2O2 acts as a reducing agent in acid solutions' and is produced by boiling ascorbic acid in H2O'
This natural production of H2O2 is enough in this reacion to add the H ion to the Harmine mole' after the oxygen has been attracted by the ascorbic acid'
The process slows down in acid solutions' but works faster in alkaline'
The stability of ascorbic acid decreases with increases in temperature and pH.
Of which means heat and increased ph makes for the ascorbic acid to attract even more oxygen'
In this reaction the ascorbic acid is oxidised' hence destoyed'
So more ascorbic acid is added to the gently boiling solution as required'

Exposure to oxygen, metals, light, and heat destroys ascorbic acid, so it must be stored in a dark, cold, and non-metallic container.


# E300 ascorbic acid,
# E301 sodium ascorbate,
# E303 potassium ascorbate,


Tannic acid, gallic acid, pyrogallic acid and formic acid are all excellent reduction agents'



Just a little heat increased ph' but still keeping below the pKa of Harmine/Harmaline so the alkaloids remain water soluble' the same as ascorbic acid'
Ascorbic acid is less soluble in hot water' and less again in alcohol'


Base with ammonia to pressipitate the THH'




Harmine/Harmaline mole to THH with foodgrade and water'

:)))



The process would take a little time an is no doubt done under reflux' so the H2O and H2O2 liberated can condence and run back into the flask'

(This satement shall have to be tryed out' ascorbic acid is quite reactive' attracting oxygen' so could possibly do the conversion quite quickly' dependant on the amount of ascorbic acid used'
Because ascorbic acid reacts with metals it is unadvisable to use a saucepan to do this experiement'
Ihave no clue if stainlesssteel wuld oxidise ascorbic acid' doubtful !

Ascorbic acid attracts oxygen very easily'


Bliss

Nobuoni +

This is only way I can work out so far without using a reactive metal to attract the oxygen from the Harmine/Harmaline mole'
I mixed up a reasonably strong solution of ascorbic acid an dropped a dirty oxidised silver spoon in it'
It stripped the oxides off in a matter of seconds an left me a with a very shiny spoon'
Ascorbic acid is used in photography as reducing agent/developer'

Anyone wish to attempt to crunch the chemistry with me ???:roll:
I believe I have answered this question'


Bliss'
 
Simple kitchen reflux'

Take a stainless steel saucepan and a pyerx dish lid' or large pyrex dish'
Place the lid upside down upon the boiling sauce pan'
and drop some ice on the lid'
The steam then comes off the cooked solution and condences' back into the boiling solution'
The ice is no nessesary but it helps grealty'

Bliss

Nobuoni +
 
Ok, pending a good yield from a rue extraction I'll probably want to try this out.

Is Ascorbic acid the only way to go with this? If so is there something I should avoid when purchasing it. I know many supplements come with certain additives that arent desirable.

Would this do?

Lamberts Ascorbic Acid 250g Powder - ExpressChemist.co.uk - Buy Online

Lamberts Ascorbic Acid Powder, supplement your dietary intake of vitamin C without the need for tablets
www.expresschemist.co.uk www.expresschemist.co.uk

Big shout to Nobuoni for the science!
 
That's a great source for food grade ascorbic acid. It's over 99% pure. I would use that or something similar like Now brand.
 
A most fascinating group of molecules' that have had very little research done on them'
A 500 mg dose of Harmine hcl effects similiar end results to high dose Ibogaine'
Except the Harmine dose has non of the after effects of Iboga' ie' being psychicaly wired out'
Has been reported to bring about abstinence from cocaine and opiates and alcohol after a single 500mg dose'
Equivilant dose for Ibogaine would be 1400mg +' but you use Ibogaine to kick substances you are going to be
flying on Ibogamines for well over a month'
Harmine seems to be way gentler but effect the same resset of NMDA receptors and dopermine pathways'
Also to add this molecule is open for "manipulations" of which no doubt other active molecules can be derived'
I shall be working close with this plant alie'
Bliss

Nobuoni +

As to other ways of converting Harmine hcl to THH' I listed some very good reducing agents including ascorbic acid'
Unless you wish to use a reactive metal' the likes of sodium or potassium and HCL acid'
Food grade reduction agents would seem to be the way to go'
Results of experimentations shall tell :)))

Pharmacutical grade ascorbic acid'
 
To add'
Syrian Rue'
No grind the seeds' boil em gently in acidic water (white wine vinegar) do this 3-4 times' at an hour a go'
Then take the seeds and ring them out inside a tee-shirt'
Combine all your solutions' reduce to 300ml'
Let settle in the fridge'
Filter by decanting through a decent coffee filter' if you let it settle properly' it filters quite quickly' unlike as of when you grind the seeds'
Add saturated salt solution to pressipitate the Harmine hcl'
Stick the container in the fridge for 2 days'
Gently decant off the salt solution' add a little fresh water to the sludge in the bottom of the container and pour into a china bowl'
Dry this product completely in a warm oven'
Bust up this resultant cake and grind it gently in a coffee grinder'
Add this powder to a flask and add a generious portion of methanol'
Warm this solution in warm water bath'
The Harmine hcl dissolves in the methanol leaving the salt behind'
Let settle and decant off this methanol into a china bowl'
Sit this bowl in a bath of hot water and evaporate the methanol' do this in the garden'
The result is a pile of very fine brown yellow crystals'

Bliss

Nobuoni +
 
what are some USA sources for methanol any way? and if its hard to get whats a decent alternative?
 
Ethanol' but you got to pay tax on it'
Methanol is easy to get' it is used to make bio-diesel' plus it is seriously cheap'
If you use "Ethanol" it must contain no "Water"'
Your object of using methanol/ethanol is that sodium chloride is practicaly insoluble in it'
But Harmine HCL is fairly soluble'

As to time'
It takes about 5 hours to wash the seeds'(this is dependant upon the amount of seeds you intend to extract) plus 2 days salting out the alkaloids'
Then you got to dry your resultant product' wash out the alks with alcohol'
Then attempt to reduce the Harmine hcl to THH'
Then you have to recover the alks'
Either by salting them out again' or by freebasing the alks with ammonia'
So you got the best part of a week'

Bliss

Nobuoni +
 
nobuoni. There is a considerable amount of reports out there of people dissolving harmalas in alcohol (and apparently acetone too) and when evapping, the product changing into a red goo (turkey red, harmala red, etc).. Apparently this product is even used as a dye. Nobody seems to know exactly what it is (maybe harmine/harmaline n-oxide? ) and if its active or not.

So whats your take on this? did you never get a red oily byproduct when evapping in methanol/alcohol?
 
Nobuoni said:
Add your Harmine/Harmaline to a strong solution of ascorbic acid and H2O' and heat gently' until the yellow colour has changed to a clear solution'
Of what happens is the ascorbic acid attracts the oxygen and the production of H2O2 donates a hydrogen'
Hydrogen peroxide H2O2 acts as a reducing agent in acid solutions' and is produced by boiling ascorbic acid in H2O'
This natural production of H2O2 is enough in this reacion to add the H ion to the Harmine mole' after the oxygen has been attracted by the ascorbic acid'
The process slows down in acid solutions' but works faster in alkaline'
The stability of ascorbic acid decreases with increases in temperature and pH.
Of which means heat and increased ph makes for the ascorbic acid to attract even more oxygen'
In this reaction the ascorbic acid is oxidised' hence destoyed'
So more ascorbic acid is added to the gently boiling solution as required'
Base with ammonia to pressipitate the THH'
Click to expand...

Seems simple enough, excellent! Is there any visual indication as to whether the synthesis has completed? It'd be nice to simply use equimolar amounts, but since the heat destroys ascorbic acid, that's probably not very reliable.
 
endlessness said:
nobuoni. There is a considerable amount of reports out there of people dissolving harmalas in alcohol (and apparently acetone too) and when evapping, the product changing into a red goo (turkey red, harmala red, etc).. Apparently this product is even used as a dye. Nobody seems to know exactly what it is (maybe harmine/harmaline n-oxide? ) and if its active or not.

So whats your take on this? did you never get a red oily byproduct when evapping in methanol/alcohol?
Click to expand...


No' no red oily gunk' but a pile of red/yellow/brown sparkly crystals'
A tiny bit' made the tongue go numb'

You got a problem salting out Harmine HCL with salt'
You can no take salt and a maoi' cos it gives you high blood pressure'
So if you salt out the Harmine and salt it out to clean it' as of when you dry your end product'
it has salt in it'

Cooked up 130 grams of Rue' four times in acetic water' no ground the seeds' or filtered' just let settle and decant' reduced to 400ml of dark red tea' of which smelt extremely strong of Harmine'
Added 300ml of saturated salt solution' stuck it in the fridge'
A couple of hours later the whole 700ml of solution had turned to a semi solid gunk' of yellow sludge' seperatedfrom the red tea'
So mixed it all up again and added 700ml of salt solution'
Now 2 litres of solution getting cold in the fridge'

(Experiment)
50 grams of Rue ground and boiled for a few hours' one serious bitch to filter'
Salted out in the fridge for one day' poured off the solution' added a tiny bit of water to the sludge and poured the sludge into a china bowl'
Stuck china bowl in the a warm oven until completely dry'
Busted up this cake and ground it in the coffee grinder'
Then added a generious amount of Methylated spirits'(Methanol/ethanol/napth/pyradine/methyl violet) of which turned instantly red'
Methyl violet turns red in acid solutions'
The methylated spirit was siphoned off leaving the undissolvables in the bottom of the flask'
Then evaporated to leave a hard cake of red/brown/yellow/sparkly crystals' of which dried completely'
This product was chucked out' cos of methyl-violet is poisonious and a skin irrative'
Shall use virgin methanol next time'
So quite possible the alcohol solution turned bright red down to the alcohol and no the methyl-violet the spirit had in it'
The only way around this would be to base the Harmine hcl with ammonia and let the base crash out of the solution' decant off the solution and wash the resultant crystals in ph adjusted water' then dry them'
Or no' a test of the resultant "RED" shall be the only way to tell if the "RED" is active'
Awaiting to see if virgin methanol turns instantly red'

So yes to red' but no to oily red'
The resultant product dried completley'

Bliss

Nobuoni +
 
Harmaline hydrochloride is yellow, not red. Harmine hydrochloride is also yellow, not red.

The red color is harmala red. No one knows the activity of harmala red. If there’s just a little bit of harmala red, it generally just coats the harmaline crystals a little making them appear reddish. If there's a lot, it looks sort of gelatin like just like this:

resource.ashx


That's harmala red forming right from harmaline after evaporation from alcohol. That pic was taken with a microscope. It’s a little hard to see the harmala red with the eyes.

It's very easy to make harmala red. Just boil some pure harmaline hydrochloride in 99% isopropyl alcohol and then evaporate it. It works every time. Keep doing it over and over and more red color keeps forming.
 
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