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DMT N-Oxide to Freebase DMT Options
 
TmC47
#41 Posted : 2/24/2009 10:21:26 PM

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Dopamine, VisualDistortion and olderROM, that all makes sense but I am not worried the spice will oxidize to any extreme extent; SWIM uses his speedy lab-technique, a very cold fridge and a desiccator for these final steps. It's the quality of the MHRB he's concerend about. Bark can lie drying in the sun for probably days to weeks, lay around for months with the vendor (even if they do claim it's fresh) and then some more moths in SWIM's place of safekeeping. In his view, the amount of spice that could oxidize during this time is much greater than the one or two days after commencing extraction. Also, since (for now) naphta is used none of this would be extracted. So, 69ron's recipe is sound. SWIM is just trying to figure out a path that would eliminate the need for an A/B and go STB *with* a reduction step tucked in there. AFAIK, Devarda's alloy creates an in statu nascendi hydrogen that is so reactive, it should reduce the oxide back to the base. It will even reduce all of the nitrate in the mix (and there's probably a lot of it in there, seeing how plants take it in in such abundance) and create ammonia from this. This ammonia will immediately leave the solution as it's so alkaline. If one was stupid enough to hold his nose over the mix (free radicals anyone?), it would be detectable by smell. Of course, this kind of reductive power could easily reduce other compounds in the mix as well, who knows what it will give rise to.
So, all knowledgeable folks here, any thoughts?
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fourthripley
#42 Posted : 2/24/2009 10:32:56 PM
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olderROM wrote:
I had an yellowish oil in a flask with water and xylene that wouldn't easily dissolve into either. However, it was SLOWLY dissolving. I added half a teaspoon of vitamin C crystals and almost immediately it dissolved. It did leave behind a nasty organish scum though but the bulk the oil instantly disappeared. I assumed that this was DMT oxide and that the vitamin C had redoxed it back into DMT.


Thats very interesting. On evap of the xylene did you find your product? if so was it solid or oil?
mistakes were made
 
fourthripley
#43 Posted : 2/25/2009 2:20:38 PM
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fourthripley wrote:
olderROM wrote:
I had an yellowish oil in a flask with water and xylene that wouldn't easily dissolve into either. However, it was SLOWLY dissolving. I added half a teaspoon of vitamin C crystals and almost immediately it dissolved. It did leave behind a nasty organish scum though but the bulk the oil instantly disappeared. I assumed that this was DMT oxide and that the vitamin C had redoxed it back into DMT.


Thats very interesting. On evap of the xylene did you find your product? if so was it solid or oil?


Scrub that; on re-reading, what happened was you acidified the aqueous solution and your goodies became ascorbic salts in the solution. Sounds like you removed some crap though. Basing the water and rextracting would give you the goodies.
mistakes were made
 
Dopamine
#44 Posted : 2/27/2009 4:00:05 PM
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TmC47 wrote:
...


Easier and quicker to do it with the A/B. You could reduce when you solvate the DMT in H2O with HCl or concentrated acetic acid over iron or zinc. Precipitate the DMT from H2O with a strong base afterwards. You should be able to get a complete extraction done in less than 2 hours if DMT precipitates well in chilled H2O as the freebase. You may want to boil off some of the H2O first or add brine before setting it on an ice bath. Use tetrahydrofuran or ether as the organic solvent if you want to get the most DMT out.
 
The Traveler
#45 Posted : 3/22/2009 6:22:06 PM

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This tek has been added to the Wiki:

DMT N-Oxide to Freebase DMT


Kind regards,

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Otiliya
#46 Posted : 8/27/2009 1:00:08 AM

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sorry to bring an old topic back. Can't a different solvent be used to get the dmt-oxide out?
I thought DMT-Oxide dissolves in DCM.


so theres absolutely no way to convert oxide into freebase form without zinc? I swear I 've read somewhere here a member said it converts with just low pH. guess they were wrong
 
West-en
#47 Posted : 8/27/2009 1:38:21 PM

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Otiliya wrote:
sorry to bring an old topic back. Can't a different solvent be used to get the dmt-oxide out?
I thought DMT-Oxide dissolves in DCM.


so theres absolutely no way to convert oxide into freebase form without zinc? I swear I 've read somewhere here a member said it converts with just low pH. guess they were wrong

Yes. You can use naphtha/heptane but it's kind of a pain in the ass. I've pulled with 50ml-heptane pulls from a solution of 1.5g DMT 5-6 times and I'm not done. Please get some real filter papers instead and pour your whole solution (after raising the pH) through them. Just remember to let it rest a bit before to let some crystals form, the fine molecular dust that appears directly after freebasing by raising the pH can actually pass through the filters.

This method is MUCH easier than the solvent-pull one and will result in MUCH more pure DMT (if there was lipids or other water and naphta-soluble impurities). Also, you won't waste naphtha and you'll get the DMT out immediately, not having to spend hours, days or weeks for the task.

I also recommend doing a hot (50 degrees) naphtha defat before raising the pH. This won't dissolve any DMT because it's in an naphta-insoluble salt form, but will get out a whole lot of impurities.

I like this whole technique (convert, defat and filter out) because it's far more efficient as a purifying method (that also converts the N-Oxide, instead of just removing it). Compare it to the popular recrystallizations! I just wonder why not more people have discovered it...
(Recrystallizations are not my best friends...)

No. A low pH won't remove the oxygen, sorry. You need something to snatch it from the N-Oxide. Using zinc for normal amine oxide reductions is standardized and a usual lab procedure for a reason! It works wonders! Wink
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Otiliya
#48 Posted : 8/27/2009 11:54:03 PM

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that's a good idea, thanks for the info. SWIM will try a clean liquid A/B definitely although is scared to spill the caustic stuff all over the place while filtering.

But what SWIM meant to say was to PULL DMT-Oxide from poor bark or a soup that's been in the garage for 2 weeks in the heat etc. Pull the DMT oxide using DCM. doesn't oxide dmt dissolve in dcm? and then do the zinc procedure guess.
 
West-en
#49 Posted : 9/6/2009 7:39:22 PM

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I think I fucked up my conversion. I had a bowl of naphtha from all previous extractions. In the bottom of this bowl there were a lot of N-Oxide. So therefore I decided to convert all the remaining DMT to N-Oxide by mixing with some hydrogen peroxide. So far, so good.

The H2O2 decomposed and I was left with a fine waterlayer, yellow to the colour, and presumable very N-Oxide-rich. So, the next step was to follow 69rons example. The water had a volume of 200ml so according to his recipe I should add 200ml 10% HCl. I only have 37% though, so I added 50ml of it. The solution got darker and a very low pH.

Since I didn't knew exactly how much N-Oxide that was in there, I decided to dump in an huge excess of zinc powder. I figured it would speed up the conversion to. So I measured up 10 whole grams of the beautiful powdered metal. Here's my mistake. Those quantities of zinc in that amount of HCl forms an reaction, an intense one. Hydrogen gas bubbled out in a way that made the water look like it was boiling and the exothermic reaction heated the solution quickly.

I don't know how many degrees it reached, but it might have been everything from 50 to 80°C. As soon as I was aware of this fact I dumped it in a water bath, but the colour of the whole mess is now black. Should I worry for destroyed potential DMT or just continue?
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voidwalker
#50 Posted : 5/9/2010 4:01:55 AM
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does anyone know if this works for 5-meo-dmt deoxidation also ? if so, what modifications to the tek would be necessary?
 
West-en
#51 Posted : 6/21/2010 12:10:40 AM

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voidwalker wrote:
does anyone know if this works for 5-meo-dmt deoxidation also ? if so, what modifications to the tek would be necessary?

Figure out at what pH most of the 5-MeO-DMT salts, that's your higher pH bound. Then check at what pH 5-MeO-DMT is endangered, e.g. goes through some unwanted chemical reaction (decomposes). That's your lower pH bound (with some safety range, of course). Information concerning these two pH-values should be available here somewhere! Smile
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Apoc
#52 Posted : 10/14/2010 8:14:31 AM

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So any word yet on the use of ascorbic acid instead of zinc? If you're a simple minded fellow like me, my thought would be to throw in a few grams of ascorbic acid and boil it with mimosa for a couple hours before basifying. No filtering, no worry about metals. Sound good?
 
foaf
#53 Posted : 12/7/2012 2:57:28 PM

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Is there any reason why zinc dust wouldn't just be used in excess?

Did any further conclusion come to pass as far as if HCl orAcetic Acid were preferred?

Thanks
 
benzyme
#54 Posted : 12/7/2012 4:49:55 PM

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is there any reason why a more widely available element, aluminum, which has a greater reduction potential, wouldn't be used?
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embracethevoid
#55 Posted : 12/7/2012 5:11:12 PM

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benzyme wrote:
is there any reason why a more widely available element, aluminum, which has a greater reduction potential, wouldn't be used?


Aluminium toxicity?

Trace amounts of zinc are cool, even good for you almost. Trace amounts of aluminium, probably not as much.
 
benzyme
#56 Posted : 12/7/2012 5:18:41 PM

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trace amounts of aluminum? we're in contact with it from everyday items;

and aluminum doesn't end up in the product when you separate with the nonpolar.
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Mindlusion
#57 Posted : 12/7/2012 5:19:15 PM

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There shouldn't be any trace metals left in your product if you clean it right,

Besides, you probably consume more aluminum then you think, we eat with it, cook with it, and drink out of it on a daily basis.

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I attempted both zinc and aluminum as reducing agents, but didn't get results.

My problem was using HCl instead of acetic acid, apparently, but I was ready to try using lithium metal
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foaf
#58 Posted : 12/8/2012 4:45:40 PM

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Quote:
My problem was using HCl instead of acetic acid, apparently, but I was ready to try using lithium metal


wasn't that the experiment where you treated dmt with peroxide and then tried to go back?

Ive read quite a few seemingly valid successful experiments where people took the orange goo or orange powder and turned it whiter and less oily using zinc.

One possible conclusion is that peroxide treaed dmt isn't the same as the orange oily material from extractions. It may oxidize or otherwise change dmt in a different way than just time and oxygen.

but again, people have gone over the stoichiometry of the reaction pretty specifically, and I can't think of a reason not to just use zinc in excess. What ya think?
 
benzyme
#59 Posted : 12/8/2012 5:40:43 PM

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of course...there's no stoichiometry with respect to zinc, it's just a catalyst for reduction.
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foaf
#60 Posted : 12/8/2012 8:09:17 PM

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It's actually a reducing agent ie electron source, and my guess is that it doesn't matter, but a couple of people had gone to lengths to put just the right amount in that's why I ask.
 
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