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DMT N-Oxide -> Freebase N,N-DMT


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#1 lysergic

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Posted 04 July 2008 - 02:58 PM

69Ron at the DMT Nexus posted this. I do not have any experience with it, but it seems interesting:

Freebase DMT N-oxide is somewhat of a pain to deal with. It’s a yellow oil that won’t crystallize. It can form after extraction and is often present in large amounts in the plant prior to extraction.

According to several sources, DMT N-oxide becomes DMT when vaporized. But some users say the effects are slightly different, so it could be that some of the DMT N-oxide vaporizes without conversion to DMT.

DMT N-oxide is insoluble in naphtha (or heptane), but soluble in water, ether, DCM, etc. If you’re plant material is old, chances are most of the DMT has oxidized into DMT N-oxide. If you’re using naphtha or heptane to extract the DMT, your yield will be very low because it won’t extract much DMT N-oxide.

Let’s say for example that chacruna leaves are used. This sometimes has lots of DMT N-oxide present. For example, in one case the alkaloid mix was 89% DMT-N-oxide and almost no DMT at all. If extracted using a naphtha based A/B extraction, you’ll end up with almost no DMT at all. The DMT-N-oxide would stay in the aqueous phase. In this case you want to either convert it back into DMT or extract it using a solvent like ether or DCM instead of naphtha.

To convert any N-oxide (such as DMT N-oxide) back into its parent freebase alkaloid, you mix it which water made pH 3 (by adding HCl acid, acetic acid, etc.) and excess zinc dust. Mix it continuously for up to 2 hours at room temperature for the conversion to be complete. The remaining zinc dust is filtered off. The pH is then adjusted to pH 9, and the freebase alkaloid is then extracted with a non-polar solvent leaving behind zinc hydroxide in the aqueous phase.

This DMT N-oxide to freebase DMT trick should be part of the initial extraction. After acidifying your extract, before doing a freebase extraction, simple add a lot of excess zinc dust and mix it for 2 hours. Then freebase your DMT and extract it into naphtha. This will greatly increase yields for most plants that contain large amounts of DMT N-oxide that would otherwise be lost in naphtha based extractions.

DMT N-oxide tends to form from DMT when exposed to air drying by a fan, especially in elevated heat. This will make your DMT yellowish and oily. If enough DMT N-oxide is present, you won’t be able to crystallize your DMT unless you freeze precipitate it in naphtha. Dissolving a mix of dry DMT and oily DMT N-oxide in a small amount of warm naphtha will cause the DMT N-oxide to sink to the bottom of the naphtha as yellow or brownish sticky goo. Mix the goo around in the naphtha to free the DMT from it. The DMT will dissolve in the naphtha and can be poured off with the naphtha, leaving behind the DMT N-oxide. Then the DMT can be placed in the freezer to crystallize in the naphtha. Don’t discard the DMT N-oxide goo! You can convert it back into DMT later once you get some zinc dust.


Might be interesting to try, if one had an abundance of oily goods that won't crystalize. Anybody know where to get zinc?
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#2 lysergic

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Posted 04 July 2008 - 03:04 PM

This process was also posted by 69ron at the DMT Nexus:

CORRECTION: the poster was quoting from page 10 of K. Trout's "Trout's notes on the genus Desmodium."

DMT and 5-MeO-DMT can also readily be converted to their N-oxides by the action of hydrogen peroxide in ethanol. (1 ml 30% hydrogen peroxide per 4 ml of ethanol) (Separates as flocculant solid.) Trituration with petroleum ether (grinding with solvent in mortar and pestle) will extract the phenethylamines, while the N-oxides remain behind in the residue.


Seems plausible....I think he meant tryptamines though (not phenethylamines).

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#3 Psilo-somatic

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Posted 04 July 2008 - 03:46 PM

I had a chemistry set when I was a kid that had a vial of zinc powder, but i'd imagine you'd need more than a gram or so... I would love to know where to get a good amount though...
...anyone?

#4 extrememetal43

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Posted 04 July 2008 - 04:19 PM

anyone know where to get DCM? never seen it at the hardware store, do u have to get it at a chemical place?

#5 lysergic

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Posted 04 July 2008 - 04:55 PM

Maybe acetone would do the trick?

#6 bear

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Posted 04 July 2008 - 10:01 PM

DCM is in some strippers though you might have to distill it to get it pure. You can buy it. It is a liver carcinogen

Zinc Dust: http://unitednuclear.com/

#7 extrememetal43

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Posted 04 July 2008 - 10:14 PM

DCM is in some strippers though you might have to distill it to get it pure. You can buy it. It is a liver carcinogen

Zinc Dust: http://unitednuclear.com/


just a question have you or anyone else ever ordered from this place or anyother chemical place? SWIM is paranoid to order any chemical from a chemical place or lab equip etc. even if its sumthin regular like a ph tester for a pool or citric acid from above place etc. I notice on this site for sum of the chemicals it requires an adult signature for delivery.

#8 cheech

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Posted 04 July 2008 - 11:18 PM

i'm skeptical, as usual.

#9 marsofold

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Posted 05 July 2008 - 11:57 AM

If the powdered Zinc thing works, it's worth knowing about.
Goo in some extractions can be problem.

Some useful chemical supplier links:
------------------------------------------------
General chemicals:

http://www.sciencela...ge/S/CTGY/10403

http://www.sciencest...Chemistry.shtml

-------------------------------------------------
Lye source I've done business with:

http://summerbeemeadow.com/

#10 bear

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Posted 05 July 2008 - 12:02 PM

just a question have you or anyone else ever ordered from this place or anyother chemical place? SWIM is paranoid to order any chemical from a chemical place or lab equip etc. even if its sumthin regular like a ph tester for a pool or citric acid from above place etc. I notice on this site for sum of the chemicals it requires an adult signature for delivery.



No one is going to bust down your door for anything on that website. The only thing that requires an adult signature is the chemicals that are strong oxidizers useful for pyrotechnics.

#11 BuckarooBanzai

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Posted 05 July 2008 - 02:42 PM

Good thread - but it is bordering on the no-no country of chemical sources. Not across the border yet and I'd like to see how this discussion develops, so tread carefully.

Again, not trying to spank anybody and I don't want to squelch an interesting discussion.

Remember the "golden rule about RCs" around here: chemistry is cool, but if you start discussing specific chemical sources, the thread will get closed and trashed...

#12 lysergic

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Posted 05 July 2008 - 03:20 PM

Any chemists care to comment?

#13 shoe

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Posted 07 July 2008 - 07:35 AM

hopefully this will boost our yeilds since some dmt naturally exists as n-oxide.

also; that seems to be all that i am getting. Can't evaporate my white spirit anymore, it just remains as a bloody liquid. its very annoying.

Also, am trying desperately to get zinc dust, but can't find it anywhere. found one site which won't accept maestro.

:(

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Posted 07 July 2008 - 08:46 AM

hopefully this will boost our yeilds since some dmt naturally exists as n-oxide.
also; that seems to be all that i am getting. Can't evaporate my white spirit anymore, it just remains as a bloody liquid. its very annoying.
Also, am trying desperately to get zinc dust, but can't find it anywhere. found one site which won't accept maestro.
:(

#1
bloody as in red? or bloody as in, you're english and pissed off :p
#2
there are a number of links in this thread. have you looked yet? :teeth:
#3
what are you using to extract? naphtha? sounds like your usin something else from your issue :eusa_thin
hmmmm ;)
#4
what is the plant source youre extracting from. the raw material. ??? and if mhrb, have you tested your source against, say, bbb, or some other well known, REPUTABLE supplier of bark...and again, if indeed mhrb, are u flouring it? or just shredding/chopping it up into pieces?
#5
nevermind all the above, have you tried defatting at all?

i think your issue is one of a few things:

either:

-bunk raw material(try a new supplier/plant...
....leaf material is a pita on more levels then one. stick to mhrb.)

-bunk solvent/reagent (use only vm&p naphtha,
and i dont think its possible to fuck up any of the tried and true mhrb teks?!) :teeth:

-someting else...im tired and going to sleep :) hope this helps some!


ps- isnt zinc used by folks in the 'metal plating' trade? :cofused: just a possible source that would keep u under the radar, well, moreso then a chemical supply house :dead: :reb: dont think for a second the alphabet boys dont obtain custy lists with as much info as u provide them at point of sale, cuz they surely must. they are gangsters and fucking intimidate and get whatever they want from the supply houses justlike they do to hydro shops to catch commercial growers that slip up and use their own credit cards etc :(

#15 Entropymancer

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Posted 07 July 2008 - 10:43 AM

i'm skeptical, as usual.


You know, you could also just do a google search rather than posting that you're skeptical of a time-tested chemical procedure without providing any reason why you think it wouldn't work. Skepticism is healthy; vocal skepticism without inquiry is asinine.




If the powdered Zinc thing works, it's worth knowing about.


It definitely works. Not that I've tried it (that would be illegal) but the procedure is a common one, and it's been known to work for DMT-N-oxide (as well as bufotenin-N-oxide) since at least 1955 (the first reference I can find is from Fish, Johnson, and Horning, 1955, J Am Chem Soc 77:5892-5895).

They actually include procedures for converting free-base to DMT-N-oxide, as well as the DMT-N-oxide to free-base DMT, since the paper was trying to definitively establish the identity of the N-oxides that were found in Yopo seeds).




DMT-N-oxide to DMT
It was further found a reduction with zinc dust and acetic acid of the oxide returned the parent base in good yield, as estimated by the intensity of the color after paper chromatography.



DMT to DMT-N-oxide
A solution of 50 mg of DMT in 2 mL of ethanol was treated with 2 mL of a solution prepared from 1 mL 30% hydrogen peroxide in 9 mL ethanol. After 2 hr crystallization was induced by the addition of ether and chilling. The granular oxide was removed and recrystallized from ethanol-ether. It proved to be hydrated, and the melting points of independently prepared samples were not wholly reproducible.



#16 extrememetal43

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Posted 07 July 2008 - 01:06 PM

How much zinc dust would one add if adding it during the initial acid soaks? My guess would maybe equal it to your expected yield but i'm thinking there's 99% of other potential oxides in the bark that can be using the zinc also.

#17 Entropymancer

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Posted 08 July 2008 - 12:12 PM

I don't think it'd be the best idea to add it during the acid soaks. Once you've pooled your acidic extracts, then it would be time for this procedure (this way the reduction potential of zinc isn't being lost on phytochemicals from the whole bark).

All the references just say an "excess" of zinc. I'd figure that means at least a gram of zinc for every 5-10 grams of bark that were used.

#18 indierail

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Posted 30 July 2008 - 10:49 PM

Damn! That explains what SWIIndierail was yammering about the other day; he kept making reference to jars with tiny crystals stuck in the middle of greenish blobs once room temperature was hit from the freezer. He doesn't always make sense being a novice as he puts it.

He told me that BBB extracted MHRB gave a whole range of DMTs (plural). He lacks in tracking all his levels (except PH; he's into saltwater aquariums so has a couple meters) but has gotten results on every run. The frustrating part is pulling a crystal garden from an ice-cold freezer and watching it turn to sick looking jello in short order. In some cases he said there are actually crystals at room temp stuck in the middle as if trapped by the substance just suspended and laughing at him.

He tells me there might even be pictures he popped off that illustrate what was referenced above.

It sounds like if he retained the goo he could recover. According to SWIIndierail he has circumstances similar to shoe's where the majority was yellow, green, brownish in color and crystal-jelly in consistancy.

I'll twist his arm for photos next time I see him and ask if he plans on trying this to recover.

#19 Shadowlord

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Posted 08 August 2009 - 08:06 PM

This is great info to have.
The current bark SWIM is working with isn't that much of a problem but SWIM has also had bark the yielded mostly yellow oil that would never become a solid. If left to dry it would become very crystalline looking. But if scraped up was just a yellow or orange goo again.
SWIM will have to acquire some zinc dust.

#20 UnlearnEverything

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Posted 08 August 2009 - 10:44 PM

Wait a second, I'm confuzzeld...

"DMT N-oxide is insoluble in naphtha (or heptane),"

If this is true, then why do naptha pulls, pull out the DMT n-oxide? Such as the case with all my friends pulls?




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