Synthesis of DMT from Tryptamine

mithyl2

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in the DMT higher yield variation, what does this part mean exactly:
'were cooled to 0°C in an ice bath over a steady stream of nitrogen.'
 

Joker_55555

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in the DMT higher yield variation, what does this part mean exactly:
'were cooled to 0°C in an ice bath over a steady stream of nitrogen.'
mithyl2Note: The reason for the low yield should be a too low amount of formaldehyde added to the reaction mixture. At least two moles of formaldehyde per mole of tryptamine is needed for complete conversion to DMT.
 
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mithyl2

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Joker_55555

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ok, so do you mean the nitrogen is introduced to the reaction vessel (aka creating a nitrogen atmosphere) with something like a canister of hyrdrogen and a hose leading to a ptfe stopcock joint like this picture:


and how is the brine made?
mithyl2Yes, or you can use a nitrogen balloon. Hydrogen, not just inert atmosphere like nitrogen, helium, Argone.
Brine is prepared with table salt and distilled water. which becomes saturated or semi-saturated.
 

huanf

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is this work?i tried :Tryptamine dissolved in methanol, adding formaldehyde solution,Then, sodium cyano borohydride is mixed slowly after it is dissolved in methanol, and then ice acetic acid is added slowly. After the reaction for 60 hours, formaldehyde and sodium cyano borohydride are both excessive, and the final reaction solution is brown color. Why?
 

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is this work?i tried :Tryptamine dissolved in methanol, adding formaldehyde solution,Then, sodium cyano borohydride is mixed slowly after it is dissolved in methanol, and then ice acetic acid is added slowly. After the reaction for 60 hours, formaldehyde and sodium cyano borohydride are both excessive, and the final reaction solution is brown color. Why?
huanf
ice acetic acid is added
Hello, you had to add glacial acetic acid 99% (cas 64-19-7)

Have you completed other manipulations described here?
The majority of the MeOH was distilled off (2000 ml collected) to the distillation flask was added 1L of 5% Aq. Ammonia which was extracted with 3x250ml of DCM. The DCM was washed with a salt solution (not saturated but still pretty strong) then the DCM separated and dried with a large portion of anhydrous MgSO4. The DCM was distilled off at atmospheric pressure and then the distillation was continued under vacuum (~1 torr now) until the dimethyltryptamine was collected. Which was recrystalized from boiling hexane with a few mls of Ethyl Acetate added. This afforded 48.8g of DMT, a 35% yield.
 
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huanf

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Hello, you had to add glacial acetic acid 99% (cas 64-19-7)

Have you completed other manipulations described here?
G.PattonYes, I followed each of the steps, and after steaming the dcm, I got an amber goo, extracted with boiling hexane, and refrigerated, I got a little white stuff that wasn't dmt. Most of the amber goo wasn't dissolved, so it wasn't dmt either. I tried it twice with the same result. Has anyone tried it this way and succeeded? Were there unspecified experimental conditions that caused the reaction to fail?
 

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Yes, I followed each of the steps, and after steaming the dcm, I got an amber goo, extracted with boiling hexane, and refrigerated, I got a little white stuff that wasn't dmt. Most of the amber goo wasn't dissolved, so it wasn't dmt either. I tried it twice with the same result. Has anyone tried it this way and succeeded? Were there unspecified experimental conditions that caused the reaction to fail?
huanfUse triacetoxy borohydride instead of cyanoborohydride because cyanoborohydride forms dangerous impurity compounds. There are research articles on the internet about this and also use chloroform instead of dichloromethane as it also reacts with dichloromethane to form an impurity and this article is also available on the internet. To extract DMT, it is better to use chloroform or ether, if you remove the solvent with ordinary heat, you will end up with a very thick brown oil, although it is DMT, it cannot be recrystallized. You can allow the solvent to be removed by fanning or placing in a room at normal temperature, in which case a yellow oil will remain (if you can crystallize this oil with hexane please report, thanks)
 

bbgateraligator

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Yes, I followed each of the steps, and after steaming the dcm, I got an amber goo, extracted with boiling hexane, and refrigerated, I got a little white stuff that wasn't dmt. Most of the amber goo wasn't dissolved, so it wasn't dmt either. I tried it twice with the same result. Has anyone tried it this way and succeeded? Were there unspecified experimental conditions that caused the reaction to fail?
huanfIt was DMT, it's just a bitch to dissolve in hexane and heptane after evaporation of DCM. You have to try to dissolve it really hard. This goo will give up eventually and dissolve. Use like 200 ml of hexane instead of 20 ml you think you should use, and heat it up nicely. Go through 2l of hexane. You will dissolve it eventually.

You can try salting out this goo with fumaric acid. Should be easier if you don't have excess of solvents.
 

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It was DMT, it's just a bitch to dissolve in hexane and heptane after evaporation of DCM. You have to try to dissolve it really hard. This goo will give up eventually and dissolve. Use like 200 ml of hexane instead of 20 ml you think you should use, and heat it up nicely. Go through 2l of hexane. You will dissolve it eventually.

You can try salting out this goo with fumaric acid. Should be easier if you don't have excess of solvents.
bbgateraligatorYes, I have tried it several times with fumaric acid, but unfortunately no sediment is produced.
 

Joker_55555

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Yes, I have tried it several times with fumaric acid, but unfortunately no sediment is produced.
Joker_333I don't know where the problem is, but when the solvent is removed, a colored precipitate remains, it has a bitter taste, it also dissolves in water, but I took the nmr from it, it had no detectable peak and it was completely damaged, can anyone help? How to get salt from oil?
 

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Tryptophan to Tryptamine​


Tryptophan (454g) was suspended in tetralin (1150 ml) containing acetone (12.9 g) and the mixture was heated to reflux for 12 hours with vigorous stirring until no more carbon dioxide was evolved and the reaction mixture became clear. The solvent was removed under vacuum, and the residue was distilled under reduced pressure to give a yellow crystalline solid.


Tryptamine to N,N-Dimethyltryptamine (DMT)​


Next, 30g of formaldehyde and 120g Tryptamine were disolved in 1800ml of MeOH, to this was slowly added dropwise 50g of NaCNBH3 disolved in 550ml MeOH. Then 14g Glacial Acetic Acid was added dropwise with stirring. The mixture was then stirred for 60 hours. The majority of the MeOH was distilled off (2000 ml collected) to the distillation flask was added 1L of 5% Aq. Ammonia which was extracted with 3x250ml of DCM. The DCM was washed with a salt solution (not saturated but still pretty strong) then the DCM separated and dried with a large portion of anhydrous MgSO4. The DCM was distilled off at atmospheric pressure and then the distillation was continued under vacuum (~1 torr now) until the dimethyltryptamine was collected. Which was recrystalized from boiling hexane with a few mls of Ethyl Acetate added. This afforded 48.8g of DMT, a 35% yield.

Note: The reason for the low yield should be a too low amount of formaldehyde added to the reaction mixture. At least two moles of formaldehyde per mole of tryptamine is needed for complete conversion to DMT.


DMT; Higher yield variation​


Tryptamine hydrochloride (10 g, 62.4 mmol) and sodium cyanoborohydride (6.28 g, 100 mmol) in a mixture of methanol (400 mL) and glacial acetic acid (11.76 g, 196 mmol) were cooled to 0°C in an ice bath over a steady stream of nitrogen. A solution of 4.20 g formaldehyde (140 mmol, 11.05 mL of 38% aq. CH2O) in 125 mL of Methanol was added dropwise to the solution over a period of one hour with mild stirring. The flask was stoppered, the reaction allowed to return to room temperature slowly, and allowed to proceed for the next 60 hours. Upon completion the pH was adjusted to 8.0 by the dropwise addition of an aqueous solution of sodium bicarbonate. The mixture was then extracted 4x with 50 mL of ethyl acetate. The combined extracts were washed once with 250mL of brine and dried over MgSO4 (15g) for 15 minutes. The MgSO4 was washed clean with another 75 mL of ethyl acetate. The solvent was reduced to 100 mL on the rotary evaporator. The hot solution was added to a 200mL beaker and covered with plastic wrap which was sealed on with a rubber band. Upon cooling in the freezer overnight, the precipitated DMT was removed by filtration, and dried in the dessicator.


Overall yield: 7.88g, 45 mmol, 67%. The mp is solid, right around 64-67°C.


Removal of N-Methyltryptamine and Tryptamine from DMT​


If you're worried about NMT/T contaminating your product just do the workup this way;


Basify the aq. reaction mix to 13-14 with NaOH. Extract repeatedly with DCM. Rotovap off the DCM and add Petroleum Ether, heat to a boil and decant the Pet. Ether from any undissolved material. Cool the Pet. Ether in the freezer and collect any precipitated solids. This will remove any unreacted tryptamine. To remove NMT you can react this mixture with acetic anhydride and seperate. I know that's quite a hassle but it's a good way to cover all the bases as far as purity is concerned.



(Rhodium site archive)
Grandthumb123Is this 37% formaldehyde
 

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Rabidreject

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This guy hasn't done this, it's an old writeup from rhodium, decades old. The first recipe has shit proportion, the second specifies 38% aqueous, but 37% in methanol what you probably have is good, even better I say. Cyanoborohydride is also not needed. Here's a better modern writeup: https://www.reddit.com/r/PsychLaboratory/comments/vm570o
bbgateraligatorThis is the synth I have been looking to follow. Iv just ordered 500g of tryptamine so I should have a good few opportunities for failure!! Haha
Although, I obviously don’t want it to, you DO learn more from it….
Have you followed the Reddit one yourself?
I also slowed down Hamilton’s synth - or at least the mad three eyed chemist that he interviewed whilst making n,n-DMT.
Some people have said that it isn’t correct - I HAVE listened to that podcast that the person talked about in the comments but I can’t remember which one it is! Is it the exploring beings on DMT one that is fairly recent??
I’m SURE at least 1 person has done this on here - I actually do not intend to produce that much of it. I would rather make other things with tryptamine tbf because there are still primary tryptamines I have not tried - which is basically why I set up my lab (boy was/is that WAY more expensive than extracting DMT!!) I also would have bought less tryptamine but to be honest, when the shipping cost is the same as what your buying it becomes rediculous so if anyone wants to try this synth shout me up and I may well send you some of the tryptamine. Or sell 50g or whatever.
I am a chemist FOR MYSELF. I DO NOT SELL DRUGS - I just wanted to make that clear…not yet ha nah jk. Been there, done that got the addictions…
 

Rabidreject

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Has anyone made a vid of tryptamine to n,n-DMT or any of the other primary amines for that matter….I obviously have Tihkal but imagine chemistry - particularly, clandestine chemistry, has come a long way since then…
I would also be really interested in what else I can make from tryptamine and how do I made DET or DiPT, for example?
It does seem kind of like there should be a video for the synth of tryptamine to DMT though…
I did UTFSE but got only adverts for the sale of tryptamine…
 

The-Hive

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Has anyone made a vid of tryptamine to n,n-DMT or any of the other primary amines for that matter….I obviously have Tihkal but imagine chemistry - particularly, clandestine chemistry, has come a long way since then…
I would also be really interested in what else I can make from tryptamine and how do I made DET or DiPT, for example?
It does seem kind of like there should be a video for the synth of tryptamine to DMT though…
I did UTFSE but got only adverts for the sale of tryptamine…
RabidrejectI’ve got a DMT synthesis in my notes
 

Rabidreject

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Basically if you have successfully performed this rxn or DET or any others that be can be made from tryptamine, please DM me. I’m more than willing to mess about a bit but ultimately if there is are any other successful primary amine syntheses from this compound please let me know….
 

Rabidreject

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It’s funny the synth I have in my notes is the one you linked to and I commented on above! Ha helps to read the whole *****ing thread right? There is also the book by Michael valentine smith -psychedelic chemistry. I know he talks about it but I think he goes the indole route…
Anyway
 

Rabidreject

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Tryptophan to Tryptamine​


Tryptophan (454g) was suspended in tetralin (1150 ml) containing acetone (12.9 g) and the mixture was heated to reflux for 12 hours with vigorous stirring until no more carbon dioxide was evolved and the reaction mixture became clear. The solvent was removed under vacuum, and the residue was distilled under reduced pressure to give a yellow crystalline solid.


Tryptamine to N,N-Dimethyltryptamine (DMT)​


Next, 30g of formaldehyde and 120g Tryptamine were disolved in 1800ml of MeOH, to this was slowly added dropwise 50g of NaCNBH3 disolved in 550ml MeOH. Then 14g Glacial Acetic Acid was added dropwise with stirring. The mixture was then stirred for 60 hours. The majority of the MeOH was distilled off (2000 ml collected) to the distillation flask was added 1L of 5% Aq. Ammonia which was extracted with 3x250ml of DCM. The DCM was washed with a salt solution (not saturated but still pretty strong) then the DCM separated and dried with a large portion of anhydrous MgSO4. The DCM was distilled off at atmospheric pressure and then the distillation was continued under vacuum (~1 torr now) until the dimethyltryptamine was collected. Which was recrystalized from boiling hexane with a few mls of Ethyl Acetate added. This afforded 48.8g of DMT, a 35% yield.

Note: The reason for the low yield should be a too low amount of formaldehyde added to the reaction mixture. At least two moles of formaldehyde per mole of tryptamine is needed for complete conversion to DMT.


DMT; Higher yield variation​


Tryptamine hydrochloride (10 g, 62.4 mmol) and sodium cyanoborohydride (6.28 g, 100 mmol) in a mixture of methanol (400 mL) and glacial acetic acid (11.76 g, 196 mmol) were cooled to 0°C in an ice bath over a steady stream of nitrogen. A solution of 4.20 g formaldehyde (140 mmol, 11.05 mL of 38% aq. CH2O) in 125 mL of Methanol was added dropwise to the solution over a period of one hour with mild stirring. The flask was stoppered, the reaction allowed to return to room temperature slowly, and allowed to proceed for the next 60 hours. Upon completion the pH was adjusted to 8.0 by the dropwise addition of an aqueous solution of sodium bicarbonate. The mixture was then extracted 4x with 50 mL of ethyl acetate. The combined extracts were washed once with 250mL of brine and dried over MgSO4 (15g) for 15 minutes. The MgSO4 was washed clean with another 75 mL of ethyl acetate. The solvent was reduced to 100 mL on the rotary evaporator. The hot solution was added to a 200mL beaker and covered with plastic wrap which was sealed on with a rubber band. Upon cooling in the freezer overnight, the precipitated DMT was removed by filtration, and dried in the dessicator.


Overall yield: 7.88g, 45 mmol, 67%. The mp is solid, right around 64-67°C.


Removal of N-Methyltryptamine and Tryptamine from DMT​


If you're worried about NMT/T contaminating your product just do the workup this way;


Basify the aq. reaction mix to 13-14 with NaOH. Extract repeatedly with DCM. Rotovap off the DCM and add Petroleum Ether, heat to a boil and decant the Pet. Ether from any undissolved material. Cool the Pet. Ether in the freezer and collect any precipitated solids. This will remove any unreacted tryptamine. To remove NMT you can react this mixture with acetic anhydride and seperate. I know that's quite a hassle but it's a good way to cover all the bases as far as purity is concerned.



(Rhodium site archive)
Grandthumb123This is the synthesis that got me interested in organic chemistry! I saw the dude with three eyes perform it on Hamilton’s Pharmacopea.

I actually ended up taking a different route in the end - I simply used the borohydride instead of making STAB….so far!
Im waiting for my vacuum desicator tomorrow and so then will be able to dry my final re-x’s from heptane.
Was surprised you used hexane - it seemed to dry real greasy to me and someone told me it’s neurotoxic.

For me, it’s getting the final product to crystalise. All the syntheses iv seen, I managed to overlook / under estimate the bloomin’ vacuum dryer!

I may well try your way if I get bored - hey do you have any info on salting it out by the way? I don’t sell and so will either have a shit load of tryptamine or shit load of DMT and I figure salted DMT would be useful for that. I don’t have much conc. fumaric acid though - does fumamaric acid work? I believe I saw someone who had extracted use it once.
 
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