Making DMT with sodium formaldehyde bisulfite and triethyl amine???

[simplechemistry]

8g of NaBH4 was suspended in cold DCM, 40ml of glacial acetic acid was added dropwise and the solution was let to stir until all hydrogen evolution has stopped.
In another rbf, 10g of 5-methoxytryptamine was dissolved in DCM. 8ml of triethylamine, 21.2g of formaldehyde bisulfite adduct and 4A sieves was added to the rbf.
The rbf was left to stir for 10-15 minutes to let the reactants condense and then the sodium triacetoxyborohydride which was made previously was added dropwise.
This was let to stir for roughly 24 hours. The reaction was quenched with dropwise addition of 15% KOH solution and a simple amine workup was done to retrieve the product which crystallised with no issues. Using sodium triacetoxyborohydride I always yield 90%+

 

[huanf]

Are you saying that the raw material for the reaction should be 5-methoxytryptamine instead of tryptamine?

 

[Never to sleep]

No you don't! Read my other comment this is a complete bullshit! You make 5-MeO-DMT instead which knocks you out like 50× more than N,N-DMT(aka DMT).

 

[huanf]

Is there a temperature requirement when you do this? Did you preheat the dce in the microwave like Hamilton?

 

[Never to sleep]

You aware that this yields 5-MeO-DMT, not DMT right?

I doubt you actually tried the procedure yourself like you claim to have done. There is NO FUCKING WAY you accidentally made 5-MeO-DMT instead and did not notice.

Cmon man. For DMT you need tryptamine. For 5-MeO-DMT you use 5-Methoxytryptamine specifically due the the methoxy group in 5-MeO-DMT...

 

[huanf]

Bro ,take easy， you have absolutely no idea what I mean when I ask you, that means “this method works with 5-Methoxytryptamine instead of tryptamine, right?" same way Hamilton said in the video that he was using tryptamine, but I saw that the solution was not the trytamine color, and I tried this procedure and it didn't work, and you mentioned the same procedure with 5-Methoxytryptamine." now we clear？ should i prove you ？！！Don't be suspicious when you don't know nothing

 

[Joker_55555]

Thank you. Only with formaldehyde 37% How to do this I think in the first step you convert paraformaldehyde to formaldehyde.

 

[Tryptamine]

Did you make Formaldehyde bisulfite adduct with 37% formaldehyde? how did it went?

 

[Joker_55555]

I am posting the reports of some people about the synthesis of this material from the sciencemadness website:

A nice addition to this topic:
75g of sodium sulfite (Na2SO3) was slushed up in 50ml of water. Then 150ml of 36% m/v formaldehyde solution was dripped into the warmed up slush of sulfite in water. After prolonged heating and stirring the mixture finally cleared up. It was then covered in foil and heated up on high temp to drive off the water. After the mixture became a white slush (at least 100-150ml of water stripped) I let it cool down and it solidified into a white rock. 50ml of ethanol was added and it was heated up once again to try to soften up the rock. It was then broken up using a spatula and dried in an oven for a couple of hours on 110C. To aid the drying I took it out and crushed the larger crumbs in a mortar.

In the end 111g (86%) of off-white powder was obtained. What's interesting is that it's flammable! I suppose heating it up releases formaldehyde which can then catch fire. Interesting. Anyways, thanks to the weight and the flammability I know this is the product. It may be slightly contaminated, but this method removes any problems with crystallization.

I, too, needed some adduct so I made it in the following way:

100 grams of paraformaldehyde was first dissolved in 170 mL of water at 60 deg. C with a few small flakes of KOH. The resulting solution was added dropwise from an addition funnel into a well stirred slurry consisting of 368.4 grams of potassium bisulfite and 108 mL of water over an hour or so. Once addition was complete, >150 mL of water was distilled off and the clear viscous solution cooled to near 0 deg. C. To the cooled mixture ~70 mL of ethanol was added. The reaction flask was shaken vigorously for a few seconds causing it to crystallize. Crystals were filtered off and the flask was rinsed with the filtrate to get everything out. The crystals were carefully dried in an oven first at 50 deg. C for a few hours to avoid having it melt into a puddle and finally at 100 degrees overnight. The product seems stable at these temperatures.

Potassium metabisulfite was used because it's what I have on hand. The product has a mildly unpleasant odor like dog food. Not quite like formaldehyde, in my opinion

 

[Joker_55555]

If we use sodium sulfite, sodium hydroxide will also be produced

 

[Tryptamine]

So sodium bisulfite method worked pretty well? I might be wrong but when Sodium sulfite is suspended in water it forms Heptahydrate but Sodium bisulfite doesn't forms hydrate I think that affected reaction I guess
also if you react aldehyde bisulfite adduct with base like NaHCO3, NaOH a reverse reaction liberates bisulfite ions to generate sulfur dioxide and sulfur dioxide reacts with water to form sulfurous acid.
but I can't figure out how to actually make Formaldehyde bisulfite adduct I think we should use sodium bisulfite not sodium sulfite
I've been researching this adduct but still no luck I found some chinese article showing how to make Formaldehyde bisulfite adduct but it was lack in detail

 

[Tryptamine]

This is raw text from Processing technology of high-transfer-rate thermal sublimation transfer paper (CN113293642)
(1)将多聚甲醛加入水中，于13-18℃条件下分批加入亚硫酸氢钠，加料完毕后升温至55-65℃反应15-25min，用NaOH水溶液调节pH＝9，冷却至室温，加入乙醇，析出固体，过滤得固体，待用。

and I found translation
(1) adding paraformaldehyde into water, adding sodium bisulfite in batches at 13-18 deg.C, heating to 55-65 deg.C after adding, reacting for 15-25min, adjusting pH to 9 with NaOH water solution, cooling to room temperature, adding ethanol, precipitating solid, and filtering to obtain solid.

 

[Joker_55555]

Yes, this is the method I posted above
I am currently testing it, you should also test it, share the result here, test it with paraformaldehyde and move on.

 

[Tryptamine]

Yeah I'm currently looking for way to get Paraformaldehyde I'm thinking purchasing on eBay but I'm not sure if I can trust vendor yet.

 

[Joker_55555]

Do you use Merck raw materials?

 

[Tryptamine]

I got one product from sigma-aldrich it was bit expensive I use chemical from chemical supplier.

 

[simplechemistry]

~30ml

 

[Joker_55555]

Hello, I did the reaction, finally the solvent was removed at room temperature, but I poured the yellow oil into hot heptane, why didn't it dissolve?

 

[SpiderDNM]

What do you mean by DMT stock ?

 

[Joker_55555]

What do you mean by DMT stock ?

 

[Never to sleep]

Ok everyone. This seems to have caused a lot of confusion. Let me clarify.

First thing's first. You don't use 5-Methoxytryptamine to make N,N-DMT(aka DMT). You use this to make 5-MeO-DMT which is a different compound alltogether, one that is much stronger.

Second this video is NOT A DIRECT TUTORIAL for DMT synthesis for a simple reason. When they filmed this episode they intentionally left out various details and steps to prevent people from using it as a tutorial. Hamilton himself pointed this out in one of his podcasts. You cannot use this video and follow step by step to make DMT. It is not even a solid foundation as it intentionally misleads you towards a wrong way of making the compound. Do actually research the synthesis prior to trying this. Making tryptamines is not really easy, not so as this video makes it out to be. Not saying it cannot be done. It certainly can. I'm just saying it is not as easy as this video makes it out to be.

 

[Joker_55555]

Yes, I understand that Hamilton did not explain his working method in detail. In general, the purpose of DMT synthesis here had nothing to do with 5-methoxy, although 5-methoxy can be made with this method.

 

[Chain react]

How was the result did you able to make DMT with that method?

 

[Joker_55555]

No.
I did not have sodium formaldehyde bisulfite

 

[Chain react]

Which podcast are you talking about? Patreon one?

 

[Joker_55555]