Anyone got an estimate on how long this should take?

Thanks.

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?

You could use IPA instead of methanol or even ethanol. Or you could use a base to freebase the Hcl's.

you dont HAVE to pay taxes on it at all... heheheh...
not with the easy still... even a retard can make ethanol with this...
http://www.home-distilli...ill-Distiller-62p600.htm

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.

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:



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.

Cheers' appreciated'
Shall know soon if absolute Methanol has the same effect as the first attempt in Methanol/Ethanol' or it was the methyl-violet that turned bright red'
The only other way around the sodium chloride would be to freebase the alks with ammonia solution'
Red or no red' it shall be tested for activity'

Bliss

Nobuoni +

HAHHA SWIMS FOAF got one of these...they are AWESOME...throw in the cheapest 50% alcohol vodka you can get..and boom a few hours later you have close to 95% ethanol...you make two mixed drinks from this stuff and you are toast!! and this comes from a serious alcoholic!! hehehe

Harmala red could even be more potent than harmaline. Who knows? I never heard of anyone testing it.

Ok, I gave the Ascorbic Acid thing a try.

A solution of ascorbic acid (300ml h2o/9g) was gently warmed until slightly bubbling then 1g of rue extract (slightly brown) was added. This was then gently heated for five hours with no colour change observed. An additional 9g of ascorbic acid was added gradually throughout heating.

Afterwards the solution was allowed to cool and then was rebased with sodium carbonate. Unlike before when the solution would turn a bright yellow this time it's a more dark/orangey colour.

Basically I have no idea what I have now. I was relying on seeing a colour change but after 5 hours it was getting late and I didn't want to leave it over night (plus it already had taken longer than expected). Once it has completely dried it will be weighed and tested sublingually.

Anyone else tried this yet?

Also does anyone know at what ph THH is expected to crash out of a solution?

The inital ph was around 3-4 but as things went on I managed to balance the ph up to around neutral, oh yeah I missed this bit by adding a little sodium carbonate. I guess that was kind of important.


Once everything's dried up I'm going to make 2 solutions. 1 of standard rue extract and the other of the ascorbic acid treated extract. I'll make them slightly acidic and then add sodium carbonate dropwise and see if they precipitate at a different ph.

I'm wondering if the slight impurities in my extract in contact with the ascorbic acid may have something to do with the darker colour when I was expecting a clear one?

Nice one bro' the only way to tell if it had any effect on the Harmine is to test it'
No got that far as of yet' still cleaning the mole from the seeds'
Keep us posted as to any difference in effect from untreated alks'

Bliss

Nobuoni +

A dry extract salted out twice' brown yellow in colour was added to 50ml of Methanol'
The Methanol went instantly red/brown'
A most deffinite red colour'
Shall leave the Methanol to do it's job' then draw it off and evaporate'
Of whatever the result is' it shall be tested sublingualy'
The red/brown colour is the same colour as the boiled seed extract' except it has no yellow to it' as in the Harmala alkaloids present in the boiled seed extract'

So possibly another Harmala alkaloid reacts with the Methanol' making the bright red colour'

A test shall prove'

Bliss

Nobuoni +

Looks like you got to base crash the alks out !

Still no info on the pKa of THH'
Harmine 7.7
Harmaline 9.8

I am guessing here by the xlog of THH' it has a pKa somewhere at 8.5 ph' ))

There are 22 alkaloids in Sirian Rue seeds'

Peganine (Vasicine)
Harmalol
2,3 - Trimethylene-4-quinazolone
1,2,3-(a-Hydroxy-trimethylene)-4-quinazolone
Oxodeoxypeganine
Oxopeganine
Tetrahydroharmine
Deoxyvasicone
2-Alkoxy-4-quinolone derivative
Deoxypeganine
Peganidine
Pegamine
Peganol
Ruine (8-Hydroxy-glucosylharmine
Deoxypeganidine
Dipegine
Isopeganidine
Vasicinone
Dyhydroruine (8 -Hydroxyglucosyl-harmaline
5- Hydroxytriptamine
6- Hydroxytriptamine
Harmol

Any one' or a combo of many could be the reason for the red in Methanol'
Only a test shall tell to it's activity'

Bliss

Nobuoni +

The thing is I never tried THH before and if it happened that only some of the extract was converted would I still notice the difference?

From all accounts a small amount should be slightly stimulating' unlike Harmine' of which is sleepy dreamy'
If the ascorbic acid had any effect' then it shall be noticable in your extract'

Bliss

Nobuoni +

SWIM's always found harmine to be fairly stimulating but understands that it's actually harmaline that makes one sleepy/dreamy. THH is more centered, like something between a mild psychedelic and a nootropic. 69ron's posted his account of the difference between the three here: http://www.dmt-nexus.me/forum/default.aspx?g=posts&t=3950. SWIM finds it to be quite accurate, though he has little experience with harmaline itself. The difference between THH and the other two is that THH lacks the mental cloudiness commonly experienced with them.