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Recovering DMT from post-freeze precipitated naphtha.

I

Indole

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Aug 9, 2011
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Let me start off by saying I am aware that there is a DMT extraction thread in PD, but I would like to see if I can get some more in depth answers here first. Mods, feel free to merge this with the extraction thread after it has gained some responses here.

Anyways, as many of you may know, the STB DMT extraction process from MHRB can leave one with a large amount of used naphtha. In my experience, this naphtha has a yellow discoloration, probably from dissolved fats from the bark. I am convinced that even after freeze precipitation in a very cold freezer overnight, there still may be some alkaloids in this solution.

A few methods that I have considered for recovering this DMT are:
1. Liquid - liquid extraction using another nonpolar solvent.
2. Super cooling the solution using dry ice.
3. Vacuum distillation of the solvent.

Vacuum distillation, while being the most practical and obvious solution, is not an option at this point.

As far as using dry ice, I have considered either dropping it directly into the naphtha solution, or placing a container of the solution into a mixture of dry ice and water. For the former method, I am concerned that carbonic acid will be generated in solution and the DMT will move into the aqueous phase. Can anyone comment on this?

Can anyone recommend a solvent for use in liquid-liquid extraction? Xylene comes to mind, but I'm not sure of its miscibility with naphtha.

Thanks for your responses.
 
Extraction is not synthesis.

The best way to "purify" naptha laced with alkaloids is probably to do an acid wash with water and then basify and precipitate shiny freebase crystals.

Without the right lab equipment I would not attempt to supercool or do a liquid-liquid extraction. Naptha is an excellent solvent for alkaloids already. Perhaps I would go so far as a cooling bath, but don't dump dry ice into your reaction mix....
 
Yeah, extract 3x into dilute aqueous acid, basify and re-extract into a smaller amount of naphtha, freeze precip.
 
Have you tried very gentle heating and using a fan over a large flat surface to evaporate off the naphtha? It's slower than vacuum distillation for sure, but I see no reason to do a more complex tech to extract what's left in solution
 
I appreciate the responses.

@sekio: the dry ice idea was suggested by a friend, I guess it was just wishful thinking.

@epsilon alpha: IME both heating of the solution and the use of a fan leads to the formation of the N-oxide which I would like to avoid. Also, my aim is to recycle the naphtha so I'm not interested in evaporating it. And it is A LOT of naphtha.

An acid wash does sound like my best bet, I'm not sure why that didn't occur to me sooner. Also, is there any way I can defat my naphtha? The cleaner I can get it, the better.
 
Using an ice-water bath would aid in the migration of the fats out of the nonpolar phase, correct?
 
Try performing the pulls on cold gunk. In my experience this prevents large amounts of fat to move over to the np phase. Excess solvent will usually result in more fats moving over and for whatever reason, so does excess base. If you can prevent as much fat as possible to move into your solvent in the first place, you'll have a much easier time cleaning up later.

I personally just evap the remaining solvent or reuse it if it is clean enough and then evap it later. The remaining low purity extract is then put into 20ml IPA (per gram) for a night along with ~300-1000mg (depending on purity) dried activated charcoal. This gets rid of most of the color, eventhough some fat remains. I used to further recrystallize this product until I got shiny white crystals, but these days I just keep the orange crystals and smoke those. They are just as good as the white ones, sometimes even stronger (go figre) and in my experience they don't put anymore stress on my respiratory tract either.

There's also another trick to remove some of the red stuff from the dirty extract... Some solvents (a hydrocarbon like heptane seems to be most people's first choice) will allow you to selectively dissolve your dmt while leaving some nasties out. I've heard of multiple people using this to their advantage and so have I. It sounds a little messy, but it works surprisingly well...
I would just pour enough hot solvent onto the dirty extract to dissolve most of it, but some will be left in a separate liquid phase on the bottom (if hot solvent is used). If you just pour the solvent off into another vessel and recrystallize you will have a surprisingly clean product.
I'm only paying 3 Euros per liter of solvent, so I never bother to recycle solvent these days (shame on me, I know) and can't give any better advice...


@sekio
The baseified water wash sounds intriguing, could you let me know how exactly you perform it? I haven't had any success with that in the past... Can you really see all the color move out?? Might be worth recycling after all if that works very well.
 
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I agree with you that extracting from cold MHRB gunk will probably lead to less fats in the nonpolar phase, but I like to get every last bit of spice out of my bark, so I usually do at least one pull after heating with a water bath at about 120 degrees F. This is where most of the fats are absorbed. In my latest extract I had a very thick layer of saponified fatty emulsion which I was sure still contained some DMT. So I did a hot pull with xylene which was very dark red and managed to pull all of the fats out. The xylene was evaporated off overnight and I was left with a deep red oil which was pretty gnarly looking. So I did a recrystallization from Heptane, as you suggested above, which cleaned the product significantly. In my opinion, Heptane is the best recrystallization solvent for DMT.

On a related note, in the past I have recrystallized my STB product from Heptane and recovered the red impurity layer that does not dissolve in the hot Heptane. Feeling adventurous, I smoked some of it (not sure if that was a good idea) and it is active, albeit subtly so. I have a feeling that this deep red oil is the N-oxide due to it's insolubility in hot Heptane.
 
Indole said:
I agree with you that extracting from cold MHRB gunk will probably lead to less fats in the nonpolar phase, but I like to get every last bit of spice out of my bark, so I usually do at least one pull after heating with a water bath at about 120 degrees F. This is where most of the fats are absorbed. In my latest extract I had a very thick layer of saponified fatty emulsion which I was sure still contained some DMT. So I did a hot pull with xylene which was very dark red and managed to pull all of the fats out. The xylene was evaporated off overnight and I was left with a deep red oil which was pretty gnarly looking. So I did a recrystallization from Heptane, as you suggested above, which cleaned the product significantly. In my opinion, Heptane is the best recrystallization solvent for DMT.

On a related note, in the past I have recrystallized my STB product from Heptane and recovered the red impurity layer that does not dissolve in the hot Heptane. Feeling adventurous, I smoked some of it (not sure if that was a good idea) and it is active, albeit subtly so.
Click to expand...
There's an excellent thread on dmt-nexus somewhere in which the threadstarter goes in detail through all the impurities and speculates about their nature a lot. It's a very interesting read! It is actually what stopped me from purifying my dimi to a glittering white. I did the xylene thing (with toluene though) thing a few times, heated a little, added some extra base, pulled once with toluene quickly and another slower pull, yielded some clear red crystals eventually one time i did this, instead of the red oil I often got in the end. Can't say what exactly I did though... The result was a substance that needed only a 30-40mg dose instead of the usual 50-60mg and which felt very heavy on the ecstatic side, moreso than the white dmt I've smoked dozens of times. The source was a different one than it usually is, but the supplier was a very well known one nonetheless.

Another time I yielded a black ball, very similar to black hash in consistency, not as sticky, smelling very pleasantly like dmt and its relatives (sort of like feces that is i suppose). I dissolved that in some Propyleneglycol, added some peg-400, buffer solution (acetic acid/sodium bicarbonate), drank that, yuk. Ive only done pharmahuasca once before when it comes to oral dmt, but thoroughly enjoyed the experience which lasted ~2 hours with a surprisingly quick onset (didnt exactly check the clock).

mhrb extractions are weird as hell, you think youve figured it all out with your years and years or bulk experience, then some variable changes unnoticed and youre at a loss whats wrong, suddenly yielding an impure or *otherwise inferior* (lol?) product or simply much less than expected despite using the same material. i didnt use to buy into the natural>synthetic story, but with this innocent plant things can vary so impressively that i wouldnt want to miss out on that getting some lab grade dmt. plus extracted dimi can go as low as 10 bucks, even at reasonable extracted amounts... if done right and the material is good.
 
CrOOK, the method I was envisioning was to have a warm naptha sol'n of the MHRB extract and then wash it (gently!) with 10% lye-water or something, then seperate and discard the aq layer... At best it pulls the alkaloids to the naptha & the protonated phenolics and fats to the water layer. At worst you get micelles and a soapy mess. Just an idea, and probably something that would take refining & tweaking to deal with exactly how fatty your bark is.

I've heard some stuff on zinc reduction of DMT N-oxide to DMT... maybe warming it in acid or something... is this acceptable content?
 
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