Hi all.

Just thought I'd share my experience of reducing yellow gooey DMT-N-oxide to white fluffy DMT freebase using the tek from the wiki:
https://wiki.dmt-nexus.me/DMT_N-Oxide_to_Freebase_DMT

550 mg assorted yellow goos saved from numerous extractions / recystalisations. Mostly DMT-N-oxide but probably contains some plant fats from an STB extraction. The goos were chilled in the fridge and scraped together into a small glass vial.

10 ml acetic acid solution (3 ml glacial acetic acid plus 7 ml H2O) was added to the yellow goo. The suspension was stirred until all solids have dissolved.

600 mg zinc powder was added to this solution and stirred vigorously. The suspension was stirred every 20 mins for 1.5 hrs. over this time the colour of the solution changed from yellow/orange to colourless, with the grey/blue zinc powder remaining in suspension.

The suspension was filtered to remove the zinc. The zinc was discarded and the filtrate was kept. 10 ml sodium carbonate solution (8 g NaCO3 in 50 ml H2O) was added to the filtrate. the solution fizzed as the carbonate neutralised with the acetic acid.

once the fizzing had subsided, 15 ml sodium carbonate solution was added with immediate precipitation of DMT freebase giving a cloudy suspension.

The suspension was then extracted with 40-60 petroleum ether (naphtha) 4 x 150 ml which was reduced down to 50 ml using a rotary evaporator (30 C water bath). A large amount of white suspension did not dissolve in the naphtha. This is presumed to be zinc oxide which precipitates on addition of the sodium carbonate but is insoluble in naphtha.

The solution was then placed in the freezer (-25C) for 3 days. DMT freebase precipitated as bright white fluffy crystals which were collected by vacuum filtration. Yield 420 mg




The theoretical yield would by around 505 mg from the 550 mg N-oxide. The 85 mg which was lost is presumed to be due to impurity of the starting N-oxide, which almost certainly contained some plant fats.

During the naphtha extraction of the basified reaction mixture, a lot of time was wasted trying to dissolve the white precipitate which remained in the water phase. This was later presumed to be zinc oxide, which is insoluble in common lab solvents. perhaps a note could be added to the wiki entry indicating that not all the white precipitate that forms on NaCO3 additin will dissolve in naphtha?

Over all I'm very happy with the outcome. I though all the goo was beyond saving, and I ended up with some of the cleanest spice I have ever seen! honestly it is super bright white and v v fluffy. The tek is very easy to follow.

Hi and thanks for tryign that out and reporting back!




Basification with sodium carbonate will produce the insoluble zinc carbonate; this is the water-insoluble, naphtha-insoluble stuff you got. What you could had done (even though I have only seen poor mention of it so far) is to leave the zinc-acetic acid-dmt solution as is; the excess zinc slowly turns to zinc hydroxide (just an overnight waiting), a strong but poorly soluble base. This would had risen your pH well enough to freebase all the dmt.

Or you could had tried to dissolve all the excess zinc metal with acetic acid (to give the water-soluble zinc acetate), then base with NaOH - this should only give dmt precipitates. Would be great if you could test whether these principles, albeit theoretically standing, also apply in practise.

Very nice work, I'm impressed with the yield from such a small starting weight.

I have some aluminium powder on order to make some thermite and was wondering if it could be substituted for the zinc to the same effect?
Is it possible that Al powder is too reactive and will have a oxide layer already formed, preventing the reaction or would it work just the same?

It does seem that powdered Al is a good reducing agent.

Thanks for the experiment!

As infundibulum said, its zinc carbonate, not zinc oxide, that precipitated.

Also one thing, while it MAY be that you turned DMT N-oxide to DMT, it may also be that you simply recrystallized DMT that was mixed with plant oils. Thats why for these experiments you need a control group, which in this case would be using part of your supposed DMT N-oxide, and do the same process except not adding zinc, to see if you also get crystal DMT out of it.

Anyways thanks for sharing

these were my thoughts exactly. In fact I'd bet that you mostly had DMT to start with.

Peace.

Well it would seem that Al is not suitable in place of Zn. After leaving a solution for 24 hours with excess Al and plenty of agitation, upon filtering and freezing for 3 days, no crystals formed :-(

Did you do a control group this time? Was it with same material?

either you had low yield to begin with, or did something wrong.
Al (-1.66 V) is a stronger reducing agent than Zn (-0.76 V).

^ yeah, good post!
it was assumed the dirty starting material was N-oxide

I had somewhere in the range of 1.5g - 2g of spice honey, I added 5ml of conc HCl to ~ 500ml H2O and redissolved the lot. There was some oily residue left over and I filtered the solution before proceeding. To the liquid I added a tsp of 200 mesh Al powder and agitated thoroughly over the next 24 hours. I decanted the liquid and filtered it, at this stage the solution was still a yellowish/orange colour however it was also cloudy. I checked the pH which was 7 and assumed the cloudiness was a freebase precipitate. I extracted with 200ml shellite after taking the pH to 13 and put in the freezer for 3 days, no crystal formation was observed.
The shellite was then poured into an evaporation bowl with 6g of plant material, which I will be interrogating shortly.

So is the consensus that Zn dust is not effective?

It's listed in the Wiki but if you read around, there seems to be conflicting information.
https://www.dmt-nexus.me....aspx?g=posts&t=7994
https://www.dmt-nexus.me...aspx?g=posts&t=34243
https://www.dmt-nexus.me....aspx?g=posts&t=1553
https://www.dmt-nexus.me...aspx?g=posts&t=23362

Is the Zn N-Oxide reduction not advised? Should the wiki be updated to at least inform people of its ineffectiveness? Am I just confused?


If it works, I have some Zn dust with MSDS of:
Metallic zinc (Zn) 98.5%
Zinc Oxide (ZnO) 1.4943%
Cadmium (Cd) 0.0001%
Iron (Fe) 0.0010%
Lead (Pb) 0.0016%
Calcium Oxide (CaO) 0.004%

The MFG lists the Maximum Lead at .15% which is pretty high, but I assume using careful separation this should not be much of an issue. Is this ok?

zinc has been described in literature to reduce dmt n oxide to dmt.. fish et al 1955 is the first paper i remember but im pretty sure there have been others.

please people when u do these experiments, have control groups otherwise we´ll never know if things are working or not

So the white precipitate would be dmt then? Or do I misunderstand?

^^^
It looks like Infundibulum is suggesting that indeed, but as soon as one bases with NaOH then the zinc acetates will goto zinc hydroxyde, and that will precipitate as white too. You will end up with zinc hydroxyde and dmt both as white precipitate. You can pull that with naphta and only the dmt goes over into the naphta, the zinc hydroxyde will not. You might think OK separation but actually the zinc hydroxyde is a little bit annoying in the pulling.

It's better to base with ammonia because it will re-dissolve the white Zinc salts back into a liquid stage just before the DMT will start to crash out. Then, you can say that the white is only DMT. This has been experimentally acknowledged.
Some texts suggest use of ammonium chloride in the process but forget about that, it is not needed for ammonium is doing the job splendidly on its own.

It is written that lye can do same re-dissolving of zinc-salts too, but in practice one needs too much lye for that too happen. It is an academic truth but of no real practical use. If using lye just deal with precipitated zinc salts during the pulling, it's doable.

It's unnecessary to let react all your zinc into zinc acetates as said, any unreacted zinc can be collected and re-used later, there's no loss. Let the zinc settle and decant the liquid trough a filter. Don't drop the settled zinc in the filter, let it sit at the bottom. The filter is to clear the liquid of trace zinc. Wash the zinc at the bottom with some water, settle, decant liquid trough same filter. Base the clear liquid as said + pull.

Hope this helps.

PS: 5 year old thread btw, with the search function more recent threads can be found.

Jees, thanks for confirming and the tips!

I used the search function, but didnt find nothing that could answer my question marks.. old threads dont scare me anymore, its just like old dmt.. or its just a part of getting older

Also I agree with JJ Spigglesworth, the wiki page on this topic (even after 5 years) is limited and could use a few more words and maybe even pics.

Will just continue to pull and maybe warm up the solution a little, as I dont have the feeling the naptha is pulling a lot. Else i'll try the second batch with a different solvent and/or base..