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

[Joker_55555]

Hello friends, have you tried the method of making DMT with sodium formaldehyde bisulfite and triethyl amine?

In this clip, Hamilton synthesizes

https://www.google.com/url?sa=t&rct=j&q=&esrc=s&source=video&cd=&cad=rja&uact=8&ved=2ahUKEwiRzLjXtLX4AhVEhM4BHQD7A_wQtwJ6BAgFEAI&url=https%3A%2F%2Fwww.youtube.com%2Fwatch%3Fv%3Dv4IC7N2gvN0&usg=AOvVaw09W-TKhI7RzU2vJQYVh1kk

 

[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]

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%+

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

 

[Never to sleep]

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%+

simplechemistryYou 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]

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...

Never to sleepBro ,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]

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%+

simplechemistryDo you make 5-meo -dmt with this method ?? In the clip, Hamilton uses dichloroethane and the fact that you are using methylene chloride does not react with methylene chloride ?? He also uses the microwave
Can you explain the extraction method more? For more details (Hamilton takes the DMT using the crystal fumarate method) thank you

 

[Joker_55555]

I also want to synthesize sodium formaldehyde bisulfite but I can not find a way to synthesize it. You have a way to synthesize this substance؟
Thank you.

 

[simplechemistry]

Do you make 5-meo -dmt with this method ?? In the clip, Hamilton uses dichloroethane and the fact that you are using methylene chloride does not react with methylene chloride ?? He also uses the microwave
Can you explain the extraction method more? For more details (Hamilton takes the DMT using the crystal fumarate method) thank you

Joker_333Dichloroethane is superior solvent for this. I just didn't have it on hand.
The reaction happens only with the end product (Tertiary amines are way more prone to attack by DCM) and at low amounts.
After quenching the reaction with 15% KOH, transfer all of it to a separatory funnel, separate the organic, wash with dilute KOH, saturated NaCl, dry with MgSO4. Distill the DCM off, extract with boiling heptane and put in freezer

 

[Joker_55555]

And 5-meo-dmt is synthesized?
I thought this method did not work on maxamine and was only for tryptamine.
Is the purity of 5-meo-dmt good?
And can mexamine chloride be used? thank you

 

[Joker_55555]

Dichloroethane is superior solvent for this. I just didn't have it on hand.
The reaction happens only with the end product (Tertiary amines are way more prone to attack by DCM) and at low amounts.
After quenching the reaction with 15% KOH, transfer all of it to a separatory funnel, separate the organic, wash with dilute KOH, saturated NaCl, dry with MgSO4. Distill the DCM off, extract with boiling heptane and put in freezer

simplechemistry.
And 5-meo-dmt is synthesized?
I thought this method did not work on maxamine and was only for tryptamine.
Is the purity of 5-meo-dmt good?
And can mexamine chloride be used? thank you

 

[Joker_55555]

Dichloroethane is superior solvent for this. I just didn't have it on hand.
The reaction happens only with the end product (Tertiary amines are way more prone to attack by DCM) and at low amounts.
After quenching the reaction with 15% KOH, transfer all of it to a separatory funnel, separate the organic, wash with dilute KOH, saturated NaCl, dry with MgSO4. Distill the DCM off, extract with boiling heptane and put in freezer

simplechemistryI also want to synthesize sodium formaldehyde bisulfite but I can not find a way to synthesize it. You have a way to synthesize this substance؟
Thank you.

 

[simplechemistry]

And 5-meo-dmt is synthesized?
I thought this method did not work on maxamine and was only for tryptamine.
Is the purity of 5-meo-dmt good?
And can mexamine chloride be used? thank you

Joker_333Ofc you can make 5-MeO-DMT using this way... why wouldn't you? Yes 96%+ purity easily. If you have mexamine hcl, you need to freebase it, extract with DCM and dry it before use

 

[simplechemistry]

I also want to synthesize sodium formaldehyde bisulfite but I can not find a way to synthesize it. You have a way to synthesize this substance؟
Thank you.

Joker_333100g of paraformaldehyde and small amount of KOH was added to 200ml of water at 70C. This was let to stir for an hour and then gradually added to a rbf with 100ml of water and 150g of sodium sulfite.
This took abit over a hour and once done was let to stir for 15 minutes. The solution was concentrated and cooled to 0C with an ice bath. 80ml of EtOH was added and the rbf was shaken to kick start crystalisation.
The crystals were filted out and washed twice with the filtrate. The crystals were dried over a few hours in an oven.

 

[Joker_55555]

100g of paraformaldehyde and small amount of KOH was added to 200ml of water at 70C. This was let to stir for an hour and then gradually added to a rbf with 100ml of water and 150g of sodium sulfite.
This took abit over a hour and once done was let to stir for 15 minutes. The solution was concentrated and cooled to 0C with an ice bath. 80ml of EtOH was added and the rbf was shaken to kick start crystalisation.
The crystals were filted out and washed twice with the filtrate. The crystals were dried over a few hours in an oven.

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

 

[Tryptamine]

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

Joker_333Did you make Formaldehyde bisulfite adduct with 37% formaldehyde? how did it went?

 

[Joker_55555]

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

TryptamineI added sodium bisulfite to 37% formaldehyde and dried it with heat. The melting point is around 190 degrees.

 

[Tryptamine]

I added sodium bisulfite to 37% formaldehyde and dried it with heat. The melting point is around 190 degrees.

Joker_333How much sodium bisulfite you used? if I want to make Formaldehyde bisulfite adduct out of 100ml 37% formaldehyde solution how much do I need?

 

[Joker_55555]

How much sodium bisulfite you used? if I want to make Formaldehyde bisulfite adduct out of 100ml 37% formaldehyde solution how much do I need?

TryptamineYou can go ahead with the molar ratio, but I poured 5 ml for one gram and then let it evaporate on the heater.
You can test this test and get the melting point and report to me

 

[Tryptamine]

You can go ahead with the molar ratio, but I poured 5 ml for one gram and then let it evaporate on the heater.
You can test this test and get the melting point and report to me

Joker_333Does sodium bisulfite reacts with formaldehyde and leave no sodium bisulfite? I'm kinda worried about sodium bisulfite residue

 

[Joker_55555]

Does sodium bisulfite reacts with formaldehyde and leave no sodium bisulfite? I'm kinda worried about sodium bisulfite residue

TryptamineWhen I tried to get the melting point of the substance, about half of the substance melts at 190 degrees, not half of it, maybe some part didn't react, I don't know why

 

[Joker_55555]

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.

TryptamineDo you use Merck raw materials?

 

[Tryptamine]

Do you use Merck raw materials?

Joker_333I got one product from sigma-aldrich it was bit expensive I use chemical from chemical supplier.

 

[simplechemistry]

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

Joker_333Exactly, you can just add sodium sulfite straight to your formalin solution and do workup as shown. Or run it formaldehyde excess and distill off the water + formaldehyde and you'll be left with with your adduct.

 

[Joker_55555]

Dichloroethane is superior solvent for this. I just didn't have it on hand.
The reaction happens only with the end product (Tertiary amines are way more prone to attack by DCM) and at low amounts.
After quenching the reaction with 15% KOH, transfer all of it to a separatory funnel, separate the organic, wash with dilute KOH, saturated NaCl, dry with MgSO4. Distill the DCM off, extract with boiling heptane and put in freezer

simplechemistryFor one gram of raw product,
How many milliliters of boiling heptane is needed ?

 

[simplechemistry]

For one gram of raw product,
How many milliliters of boiling heptane is needed ?

Joker_333~30ml

 

[Joker_55555]

~30ml

simplechemistryHello, 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?