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DMT Extraction from Mimosa Hostilis problems

ros1816

ros1816

Bluelighter
Joined
Mar 11, 2014
Messages
106
My girlfriend is a PHD Chemistry student and is attempting to perform a DMT extraction on Mimosa Hostilis Root Bark.

We are using this technique http://www.ayahuasca-recipe.com/dmt-from-mimosa-hostilis-rootbark

My girlfriend decided to use hexane instead of naphtha. We also soaked the bark in sodium hydroxide for 24 hours (so longer than the tek). Everythingelse is unchanged.

We are at the stage of separating the organic layer from the aqueous layer.

In her words:

"It seems to be going a lot slower than expected. (I would expect the hexane to rise to the top within a few minutes but it's been 2 hours and is only now starting to form a very small layer).

I wouldn't expect hexane to form a stable emulsion."

Can anyone shed any light on why the process isn't working/is taking so long?

[[If anyone were to suggest an alternative tek unfortunately we can't perform "noman's tek" as we don't have a freezer!]]
 
Add more NaOH.
That should help break your emulsion...why, though, wouldn't a "PhD Chemistry student" know that?
 
When you saponify the fats from mimosa, you make.... soap! So of course it will form a semi-stable emulsion.

Salt it out by adding table salt til no more dissolves & mixing again. Or just add more hexane, gently swirl it around, & remove the layer.
 
It's legit - she really is a top PHD student at one of the foremost academic institutions. Its ridiculous - im not impressed at all! (she messed up the cook on 2 grammes of ketamine once too - although to be fair she was on ketamine. She also failed to make crack [we did it for a laugh] and blamed it on the coke being of such poor quality to start with!). It's an interesting situation trying to communicate this bcos Im relaying things thru her - she is too busy to post, is terrible at explaining things [but i still love her], and I have the world's worst understanding of chemistry/anything practical. Anyway ...


Possible ways she fucked up:
-She should have used naphtha not hexane.
-She may have soaked it in NaOH for too long (we left it for about 34 hours)
-She mashed it up too long (she mashed the already well broken down bark+NaOH mixture for 30 minutes)


Possible solutions:
-Adding Naptha instead. She has gone to buy some lighter fluid - she says that will make the top layer form more quickly. Is this advisable?
-Add more sodium hydroxide - although the hexane has already been added so it is possibly too late?
-Add salt?


@phuckingnutz what different teks do you recommend [that don't involve freezing - we don't have one] - you've been doing this for years no?
 
Just goes to show that it's "Piled Higher & Deeper".... just because you have an education these days, doesn't mean you're qualified to work in your field. I have dealt with Ph.D chemists who couldn't figure their way out of a wet paper bag and totally uneducated folks that could be the next Walt White.

Three things will help here: salting out the organic layer, increasing work-up volume with more naptha or whatever, or being patient. A defat would have helped too, but it's too late for that by now.

Hexane is basically a more highly refined naptha - it works excellent for STB. Soaking it for days is fine, so is mashing it up.

You just have to accept that an emulsion can form and not shake the ever living shit out of it. Mix the organic layer and the aqueous layer *gently* when you add them. Swirl it around. DON'T grab the container and shake like a Shake-Weight. Otherwise you'll have to let it sit for a day or more for the emulsion to die.

Again, adding salt will increase the ionic strength of the aqueous layer and force the hexane to break its emulsion. It's the most trivial way of doing it and can also prevent future emulsions from forming.
 
I would also advocate heating the solution just a bit, to, say, 60 degrees Celsius. As has been previously said, adding more NaOH and/or table salt will make the black layer more polar and thus will aid in separation of phases. In my experience this separation issue arises when there is too little aqueous phase or too much mimosa powder, especially the Brazilian one.
 
Isn't table salt mostly effective because it helps bind any polar moieties to the salt ions? I'm not really sure if that is what you meant sekio.

And sure, heating it up by running hot water over a separation funnel should be somewhat effective, it just speeds everything up a bit - as a rule of thumb.

Napthta, from what I understand, contains hexane and very similar hydrocarbons like maybe heptane and branched ones of similar MM.

Ehh I think lighter fluid is butane, not sure if you want to add that - also it seems like a "good" way to bust your funnel. Lol I did that once generating too much CO2 from carbonic acid, you do that shit once and then never again.
 
Lighter fluid is naphtha AFAIK. Worked well for me, tried different brands - all were equally effective.
While performing my very first extraction I accidentally bought kerosene in place of naphtha and still managed to get it done...just took 3 days to evaporate lol. So as long as it is nonpolar, it will work ;)
 
Yeah no, I still recommend against butane (which is what lighters are filled with in my country IIRC, tho maybe not zippo's which take gasoline or sth). Butane may evaporate a little too readily to put it in a funnel and swirl it around. It is a gas under normal conditions!
You can check if it's butane by putting it in a ziploc baggie and holding it in your hand. If the heat from your hand makes it boil, it's butane.

Butane may be great for making awesome hash oil, but it can be dangerous to work with.

wiki said:
Butane is also used as lighter fuel for a common lighter or butane torch and is sold bottled as a fuel for cooking and camping
Click to expand...

Again, don't know about your country or specific shop.

Not all non-polar solvents are okay, especially if they don't evaporate well or cleanly. There can be toxic compounds in them and some are entirely toxic by nature...

Ingestion of kerosene is harmful or fatal. Kerosene is sometimes recommended as a folk remedy for killing head lice, but health agencies warn against this because it can cause burns and serious illness. A kerosene shampoo can even be fatal if fumes are inhaled.[34][35]
Click to expand...
 
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I have personally tested Zippo, Ronsonol, and Newport lighter fluids. All work equally well, but Newport being the cheapest is my choice usually.
I have also successfully used toluene and xylene, but these are REALLY smelly and take much longer to evaporate than the mentioned lighter fluids. Yet those solvents are much cheaper.
Anyway, if I had hexane I would just stick to it.
 
Toluene and Xylene should be great to make red jungle spice, but yeah you have to put extra effort into their evaporation (fanning etc), they are carcinogenic.
 
Hi, this is ros1816's girlfriend posting. I totally admit I should have thought of adding salt- I've used that trick many times before when I was working in industry lol. I would like to point out that I was a bit stressed at the time because ros1816 was freaking out and yelling 'WHY HASNT IT WORKED AAARGH' and I was also trying to leave the house to go and invigilate an exam. We've done another extraction now using white spirit in place of hexane, should have though of that sooner too, much cheaper. Oh well, it's all a learning process. Thanks everyone for your advice! Will report back when the white spirit has evaporated
 
This is mrs ros1816 again. The white spirit has mostly evaporated and there is what looks like a good lot of crystals forming, still must be around 10 mL of solvent left though which must be a saturated solution. That got me thinking, what would really be the best solvent to extract DMT? Looking at the chemical structure I would guess it's lipophilic but polar. If I was going to extract it in the lab I'd probably use ethyl acetate or DCM rather than hexane. Definitely wouldn't use DCM in a non-fume hood environment though.

What I'd like to do is TLC a bit with 50/50 EtOAc/hexane, and see what the polarity is like. That would involve nicking some TLC plates and ethyl acetate from the lab which is something ros1816 is dead against me doing!

One more thing I've been thinking about- and maybe this is so obvious it doesn't need saying- but that tek we linked to doesn't say anything about safety. Just in case there is someone reading this who doesn't know about this stuff, I would always wear a labcoat, goggles and gloves when handling any of these chemicals. Perhaps it goes without saying but perhaps not!

Sorry to bang on about geeky chemistry stuff.
 
Hexane is reported to be highly selective for DMT freebase and is generally employed for further purification of the product via subsequent recrystallization cycles. For initial extraction naphtha a.k.a lighter is more commonly used. It evaporates fast and one can freeze precipitate the DMT freebase out of it, which is a major plus since it is not possible with toluene/xylene and related solvents in which DMT remains still very soluble even at freezing temperatures. Xylene/toluene, on the other hand, have the advantage of not needing to be heated to catch up the majority of DMT, while yields with naphtha are highly dependent on the temperature of the solvent; pulls made at 20 degrees vs 60 degrees Celsius differ to a great extent. Yet heating the solvent makes plant fats more likely to migrate into the NPS, thus contaminating the final product if defat procedures had been performed beforehand.
 
afer said:
Hexane is reported to be highly selective for DMT freebase and is generally employed for further purification of the product via subsequent recrystallization cycles. For initial extraction naphtha a.k.a lighter is more commonly used. It evaporates fast and one can freeze precipitate the DMT freebase out of it, which is a major plus since it is not possible with toluene/xylene and related solvents in which DMT remains still very soluble even at freezing temperatures. Xylene/toluene, on the other hand, have the advantage of not needing to be heated to catch up the majority of DMT, while yields with naphtha are highly dependent on the temperature of the solvent; pulls made at 20 degrees vs 60 degrees Celsius differ to a great extent. Yet heating the solvent makes plant fats more likely to migrate into the NPS, thus contaminating the final product if defat procedures had been performed beforehand.
Click to expand...

I see. So do you think a more polar solvent like ethyl acetate would also extract more of the unwanted stuff? Hexane is likely the best solvent then for the really pure stuff. I still have about 600ml of hexane- I could save that for doing recrysts. It's a pity the stuff is so expensive, about 10x the cost of white spirit.
 
I have never used ethyl acetate so can't really comment on that, but it does appear that it will draw more of unwanted impurities along with the DMT. Personally I have found the simplest way to get reasonably pure crystals is to use Straight-To-Base tecs, add plenty of salt, then heat the entire solution along with naphtha to around 40-50 degrees Celsius (this is the magical number when DMT is highly soluble in NPS, but plant fats are not yet), do 3-4 pulls, and then evaporate the solvent. This worked best with Brazilian mimosa; Mexican mimosa IME is quite fatty and requires previous defats (either dry defats of the bark itself with plenty of NPS or defats of acidic solutions containing DMT salts..but this essentially means that the tec is converted to Acid-To-Base which complicates the whole procedure and IME gives less yield that Straight-To-Base).
 
Hexane and other alkanes are the best for M. hostilis and friends, DCM reacts with DMT to form N-chloromethyl-NN-DMT chloride (!) and is less selective as a solvent anyway. Chloroform & EtOAc are OK if you don't mind pulling lots of other shit out too.
 
So we've done 3 extractions now- the first one (not enough solvent) netted 100mg, the second (lots of solvent) 1.3g, and we haven't weighed the third one yet but it looks like a few hundred mg to me. The crystals are yellow and have two distinct crystal forms- this worried me a bit until I found this paper http://journals.iucr.org/b/issues/1972/10/00/a09347/a09347.pdf which describes how DMT crystallizes in two different crystal modifications, both monoclinic but with different numbers of molecules in the unit cell. Unfortunately the paper doesn't have any nice pictures.

I want our crystals to look like these
407502250-DMT_Crystals_10.1.jpg

I can see the same shapes but they are yellow. Both of us have tried smoking a bit of this crude product and agree that it is definitely DMT but not very strong. People have mentioned recrystallizing multiple times- how necessary is this? In my experience as a chemist, if you do it properly you only have to do it once.
 
Yellow color is due to some miniscule impurities, e.g. fats and waxes. These do not consideably detract from the experience and personally I would just use the product as such. As long as it is crystalline and not some gooey mess it is good enough to smoke IMO.
 
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