DMT Precipitation via Vinegar

[Takanuva1999]

Hi y'all!

So I'm in the middle of a dmt extract, and big surprise, I have some questions...

I pulled a layer of naptha off my basified MHRB solution, and proceeded to filter it to remove any solid impurities. Next, the naptha + freebase went into a separatory funnel, where the naptha was washed with a 200mL solution of sodium bicarbonate x3. This was followed by x3 washes with distilled water (200 mL) to remove any excess sodium bicarbonate that might have made it into the naptha. The final step was to perform 200mL pulls of vinegar (aka 5% strength acetic acid) x3 from the naptha solution. Then, the vinegar pulls should be evaporated to yield dmt acetate.

This is the step I'm currently in, and the evaporation should take a couple days to complete. However, I'm concerned about the vinegar's total lack of color. The naptha was yellowish when it had the freebase in it, and definitely got more clear after the vinegar washes, but the vinegar remains colorless. Is this normal?

Possible explanations I've thought of so far, but can't verify:
1. too low of a concentration to be visible as of yet
2. dmt acetate isn't visible in vinegar solutions?
3. the sodium bicarbonate or water washes pulled off the dmt - seems unlikely, considering neither should provide enough acidity to convert the freebase to a salt and allow it to move into the water layer
4. General stupidity? :?

 

[Brennendes Wasser]

Greetings to Metru Nui fellow Toa - any particular reason why you indeed wants DMT acetate instead of DMT?

Evaporating the acetic acid will take quite some while ... and you can only conveniently use it for oral consumption.
Freebase DMT still has an exceptional shelf life and can be used in any way that DMT acetate can be.
If you still insist on getting a salt:

Much easier and 100 % conversion is this way ...

Grab your DMT in Naphtha and throw FASA on it. Stirr while adding the FASA and then leave it for 1 day in the fridge, with the container being closed perfectly. Then decant everything and you have DMT Fumarate. Its basically the same like DMT Acetate.

Regarding your questions:

As you still have not evaporated it completely, I would not be nervous so far ... besides the low coloration there is no hint that anything went wrong.

1. + 2. If the total volume of acetic acid is higher, then this will indeed be something to consider. Also some components have a huge change in coloration strength at different pH-levels and thus different protonation levels, like most regular Dyes. Still, DMT does not contain the typical dye structure units with delocalized electrons in an aromatic system, but still coloration may vary between FB and Acetate.

3. I never did a wash like this, but you can test yourself if this was the error:

Create the same Sodium Bicarbonate solution again and measure pH - if its lower than 9 you may get a risk of removing some DMT from your solution.

4. :!:

 

[downwardsfromzero]

My feeling is, firstly, that DMT acetate solution need not have any coloration at all. Some brands of vinegar contain a preservative (sodium metabisulfite) that could theoretically decolourise the DMT freebase solution in naphtha as, again, that need not display any coloration on account of its actual DMT content either. Really pure DMT crystals can be quite colourless.

Secondly, I agree with BW that washing with sodium bicarbonate followed by distilled water could be reasonably expected to causes yield losses. One wash with sodium carbonate should suffice and IMO washing with pure water after that is unnecessary and likely to be detrimental in terms of yield.

 

[Takanuva1999]

I've already experimented with dmt freebase, and wanted to try and make a salt form (planning on doing a harmala extract to go alongside), so that's pretty much the only reason I'm doing this Also, I'm trying to avoid any leftover residue from the solvent, which happened last time I did a full evap of my naptha.

I found this link regarding the loss of product through the water/sodium bicarb pulls, but it doesn't suggest a significant amount of product is lost...

Does washing solvent layer with water reduce yield? - FAQ - All your basic questions and answers - Welcome to the DMT-Nexus

I guess I could have lost some to the water pulls, but the difference in pka (dmt - 8.7, sodium bicarb 8.2) is marginal. It's been a while since organic chemistry, but if I recall correctly, a difference of 1 between pka and pH means only 10% of the dmt is protonated - a difference of .5 should be less than 5% loss for each sodium hydroxide pull.

Still evaporating the vinegar... down to about half volume, no sign of color yet! In response to Brennendes Wasser, I have a hot plate/stirrer combo that makes evaporation pretty easy. With regards to your proposed method, trust me, if I had access to fumerate, I wouldn't be doing all this method:wink:

 

[Takanuva1999]

Update on DMT Acetate:

Looks like y'all were right.. I didn't see anything in the solution until it was almost gone, at which point I collected around a gram of a crystal/wax. It actually looks a lot like THC concentrate, and I was wondering if anyone knows the vaporization temp of dmt acetate? In theory, I'd imagine it has a lower vaporization temp than most dmt salts, as acetate is a much weaker proton donor than chloride, citrate, tartrate,etc..

Mostly just curious, since the primary focus of this extract was to achieve a more bioavailable salt. Not really planning on dabbing it, as it still smells a bit like vinegar. I still need to test the melting point against the literature, but can't find exact data for the acetate salt However, I'm not super worried about excess acetate as it has a pretty low melting point and probably came off during the heating/evap combo. If there's interest, I might also be able to upload some pictures of the final product later on.

 

[Brennendes Wasser]

I was wondering if anyone knows the vaporization temp of dmt acetate?

It was stated somewhere that you can indeed smoke those, even though salts should vaporize way too high and mostly cause combustion/degradation. So it was only reported to be a little harsher, but not caustic at all.
Still it seems there is not any additional info as there is no reason to dwell deeper into that as Freebase is just better at everything converning vaping :d

the primary focus of this extract was to achieve a more bioavailable salt

Dont be fooled by the fact that salts are water soluble and the body and its metabolism relies completely on water as a solvent. The bioactivity of charged compounds is indeed lower as regular metabolism pathways include quite some steps with diffusion through mucous membranes and this is highly slowed down or even permitted for ionic stuff.
In the example of 5-OH-DMT it was stated somewhere that the Fumarates are much weaker when administered intranasal / sublingual compared to freebase. But you may try it out!
I can say DMT Fumarate hurts in your nose for 30 minutes, even though it should dissolve instantly and be transported throughout your body within minutes ...