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help...what happens to DMT oxide during Fumarate conversion?

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closet-chemist1010

closet-chemist1010

Rising Star
Hey nexus, i have been searching and cannot find a definitive answer.

A couple of years ago i did a Very large extraction, which is a bit of good news and a bit of bad.

good news is as MHRB became hard to find i have a pile of spice.
Bad news is even in the airtight container, after this much time, and the jar being opened on many occasions. My spice is turning yellow and brown, the whole stash.

So my question is, Is it too late to turn my pile of Freebase spice into fumarate?
whats happens to the DMT oxide during the conversion if i were to go ahead with the conversion

I future ROA will be IV as my throat cannot handle the spice, so purity is main concern.


And while we are here i'll quickly ask about solubility. If im going to lose the dmt oxide anyways, is there is a simple way of dissolving either of the two in a solvent without the other? so i can do a fumarate conversion on the dmt freebase only?

Your thoughts and experiences are much appreciated!
 
Dmt n-oxide is water soluble as I recall. You can seperate the two that way. Not only that but there is a way to convert dmt n-oxide into dmt freebase by adding zinc. :)
 
If you do the FASA way, some of my tests seem to indicate n-oxide will mostly stay in solution while the DMT fumarates will precipitate, but this needs further confirmation (it might be that it was the plant oils in limonene that kept the n-oxide in solution in the tests, but doing FASA on already-purified dmt might not be the same).

Theoretically, there can be such a thing as DMT N-Oxide fumarate, but AFAIK we have not seen any proof that it exists as such, or how it would behave.

If you do FASW or any other acqueous salting, then n-oxide will be in the water layer together with the DMT.

Either way, it also seems such oxidation is more superficial according to some tests. Also n-oxide should be active too, so maybe not necessarily unwanted.

You can always do a couple of recrystallizations as a freebase and/or with FASA.

Please be careful IVing, make sure your solvents are USP grade or similar, that everything is sterile, correct dosages, setting, etc. FAQ has an entry on DMT IVing with a good link on safe IV practices.

What dosage are you considering use? Will you have a sitter? Got previous IV experience?
 
First things first, thank you for the concern endlessness. I'm a very responsible person and would never venture into any ROA or any substance without many hours of prior research Into the matter. I will read the FAQ on IVing extensivly, but do have knowledge on the subject already.

Can you specify what You mean when u say the oxidation is superficial. Does this mean the browning of my spice is not oxidation but something else?

Du57mi73 thanks for the reply. But from the reading I did it seems zinc is a Bad reducing agent and this procedure didn't actually work. Correct me if I'm wrong though, this is just the reading I did.

But both of these things support each other because if it turns out the darker spice isn't actually dmt oxide, then a procedure aimed at converting oxides to normal freebase wouldn't work.

All input is appreciated. Sorry if my spelling and grammar is terrible I'm on my phone on my lunch hour lol and the forum doesn't display too well on my phone
 
My comment on superficial oxidation was because of some DMT I left to purposely oxidize, versus a control I kept in the freezer, and after a couple of months, the 'oxidized dmt' was reddish and waxy while the other remained white and crystally. So when testing both, there seem to be only a small amount of n-oxide actually formed, which was surprising to me. My guess was that the change in color is a superficial oxidation, happening in the outer layers of the crystal formations, but not affecting the bulk of the dmt.

Of course, this was a single experiment, which would be interesting to repeat, but at least its some data we can consider.

In the case there is n-oxide, zinc reduction should work well.

Thanks for reassuring on the safety issues.
 
OK I'll have to do some reading up on the zinc reduction. Endlessness I have been reading great posts of yours for years here on the nexus, so have a level of trust on your judgment. Do you think a safe way to proceed would be to do a recrystallization. And if I get a large difference in yeild its safe to say the oxide was removed by the process (spice was very white 2 years ago) I am not familiar with the solurecrystallization of the oxide as of yet so do not know if it will be removed through a recrystallization. And then proceed with a FASA? The solvent left after a recrystallization could be evapped. Contents then used in a zinc reduction
Technique?
And what if no noticeable change in yeild is seen? Do you think it would be safe to perform a FASA on what we think is DMT oxide and have that in my final product?

Thanks for all the help so far
 
Hey :)

N-oxide will probably not be very soluble in naphtha, so recrystallizing it a couple of times should eliminate it (along with other possibly unwanted impurities).

Then dissolving in acetone and precipitating with FASA, and washing the fumarates with cold dry acetone should help cleaning it up further.

You could try doing a zinc reduction on left overs from the freebase re-x to see if you get anything out, but I definitely would try to have a 'control group' to see how much the zinc reduction is actually doing anything. So you could divide the leftover goo in two parts, and put in two different jars. Add some vinegar to both jars to dissolve the goo, to one jar you add excess zinc (a small spoonful ? ), to the other you dont. Let it react for some hours, filter both jars, add base to both jars, pull both basified jars with naphtha, evaporate them separately, compare what you have :)

As for 'whether its safe if no noticeable yield is seen', safe for what? For ingestion? Well regardless if 'yield changed or not', I'd say if you follow the points mentioned lower down the first post here, it should definitely be reasonably safe to vaporize. Regarding to IV, its a more delicate situation I guess because of added risks of IVing, and since I have no experience at all with that, I dont feel Im the most appropriate person to tell you about it.
 
I recently have some experience with this, I believe that DMT N-oxide will form a fumarate salt. I had done a xylene extraction of ACRB, removed the NMT with dry ice, then FASA'd out the fumarates. This resulted in off-white crystaline solids that were then redissolved in water. I added NaOH and the DMT precipitated. I did 5 pulls with naphtha, but a large quantity of a yellow oily layer was still stuck between the water and naphtha and didn't seem to be very soluble in either. On a hunch, I assumed it was DMT N-oxide and sucked it up and redissolved the goo in vinegar. I added zinc powder and within a hour, the solution had changed from piss-yellow to nearly colorless. This solution was then based with NaOH and several pulls with naphtha were done, leaving behind no yellow oil and yielding white DMT on freeze precipitation.

From this, I think it's safe to assume that the yellow oil was DMT N-oxide and not a primary or secondary amine (i.e. NMT), or regular DMT. Because the material had already passed through a FASA stage, I'm pretty sure that the N-oxide will precipitate as a fumarate salt.

To the OP: All you should have to do is take your oxidized DMT, dissolve it in vinegar, then add excess zinc dust. The conversion is very fast (<30 minutes) if your zinc is a fine powder, just wait for the solution color to change. Filter out the zinc and do a standard STB extraction on the resulting solution.
 
ok thanks guys those posts together give a wealth of information to help me proceed. Arcologist that was exactly what i was looking for, so for my last(hopefully) question.

should i just dump my whole pile of spice into vinegar? and add zinc, or should i attempt to separate the oxidized spice first and only perform the reduction on the dmt oxide?

again thanks so much, i just want to explore as many options as possible
 
arcologist said:
I recently have some experience with this, I believe that DMT N-oxide will form a fumarate salt. I had done a xylene extraction of ACRB, removed the NMT with dry ice, then FASA'd out the fumarates. This resulted in off-white crystaline solids that were then redissolved in water. I added NaOH and the DMT precipitated. I did 5 pulls with naphtha, but a large quantity of a yellow oily layer was still stuck between the water and naphtha and didn't seem to be very soluble in either. On a hunch, I assumed it was DMT N-oxide and sucked it up and redissolved the goo in vinegar. I added zinc powder and within a hour, the solution had changed from piss-yellow to nearly colorless. This solution was then based with NaOH and several pulls with naphtha were done, leaving behind no yellow oil and yielding white DMT on freeze precipitation.

From this, I think it's safe to assume that the yellow oil was DMT N-oxide and not a primary or secondary amine (i.e. NMT), or regular DMT. Because the material had already passed through a FASA stage, I'm pretty sure that the N-oxide will precipitate as a fumarate salt.

To the OP: All you should have to do is take your oxidized DMT, dissolve it in vinegar, then add excess zinc dust. The conversion is very fast (<30 minutes) if your zinc is a fine powder, just wait for the solution color to change. Filter out the zinc and do a standard STB extraction on the resulting solution.
Click to expand...

Thanks for sharing the experiment :)

But I wouldn't yet conclude anything about n-oxide if you didn't at least have a control group in your process, when doing the zinc reduction. Better to divide the supposed n-oxide in two, and do the exact same process except one of them without adding zinc, and see what one gets in both cases. Otherwise you can't rule out that it was a simple re-A/B which was responsible for cleaning up the DMT. Also solubilities might not necessarily be indicative of it's nature, since for example jungle spice which was washed with naphtha still shows significant DMT. Might be related to different impurities and saturation changing the solubility of compounds in solvents.
 
^exactly - Definitely use controls, otherwise such claims are to be taken with extreme caution. We had quite few pains with people claiming that colour changes actually mean something (they may, or they may not), so any colour changes must be interpreted with severe caution. There are other reasons why separating the yellow oil and doing a mini A/B to it might have helped you pull more spice, aside from putative reductions.

We are not trying to be anal with you, but since the Nexus has a strong scientific front, you should expect a high level of scrutiny. We want claims to be supported with something more solid than colour changes and naphtha pulls. TLC, for instance, would easily tell you if there is any dmt oxide in your FASAs and if this could be reduced to dmt.

Very interesting experiments non-the-less!!!
 
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