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✅The technique is suitable for the synthesis of popular tryptamines from TIHKAL. For example, replacing diethylamine on dimethylamine (3:20), you will receive DMT.

⚠️The air temperature in the laboratory should not exceed 10°C.
☣️Exhaust ventilation, respiratory and eye protection.

⚙️
  • Beakers 1000, 500, 250 and 50ml
  • Filter Flask 2000ml
  • Flat-bottomed flask 29/32 2000ml
  • Reflux condenser 29/32
  • Drop funnel 500 and 60ml
  • Glass funnel 100 mm
  • Schott funnel 60 mm
  • Buchner funnel 100 mm
  • Long-probe lab thermometer
  • Magnetic stirrer
  • Lab support stand
  • Rotary evaporator
  • Hot plate with temperature control
  • Single stage vacuum pump
  • Filter paper
  • Mortar and Pestle
  • Generator of hydrogen gas (dry hydrogen chloride HCl)
  • Lab spoon spatula (stainless steel)
  • Glass stirring rod
  • Crystallizing dishes 60-200mm
  • Litmus test paper (pH 0-12)
  • Syringes 20ml (x4)
🛢️
  • Indole 20g
  • Oxalyl chloride 22g
  • Diethylamine 40ml
  • MTBE 1800ml
  • Methanol 750ml
  • LiAH 19g
  • Anhydrous dioxane 1200ml
  • Wet dioxane ~10-20ml
  • Anhydrous MgSO4 20g
  • Dry hydrogen chloride HCl (gas)
  • Benzene 250ml
  • Diethyl ether 300ml
📑

Stage 1/4

Preparation of 3-Indoleglyoxylyl chloride

20g indole + 240ml MTBE
22g oxalyl chloride + 240ml MTBE

Stage 2/4

Preparation of N,N-diethylindol-3-ylglyoxylamide

3-Indoleglyoxylyl chloride + 1200ml MTBE
Rm + 40ml diethylamine

Stage 3/4

Reductive amination of N,N-diethylindol-3-ylglyoxylamide to N, N-diethyltryptamine via LiAH

19g LiAH + 350ml anhydrous dioxane
19g N,N-diethylindol-3-ylglyoxylamide + 350ml anhydrous dioxane

After 26h used 10-20ml wet dioxane

The filtrate is dried over 20g anhydrous MgSO4

Stage 4/4

Crystallization of N ,N-diethyltryptamine hydrochloride (DET)

Oil (Freebase) + 100ml diethyl ether
Bxj4qsT1HX

STAGE 1/4​

(0:53-1:10) - 20g of ground indole (1) dissolves in 240ml MTBE
(1:11-1:20) - 22g oxalyl chloride (2) was dissolves in 240ml MTBE
(1:25-1:50) - The oxalyl chloride solution is placed in a dropping funnel and with vigorous stirring, dropwise, within 30 minutes is added to the indole solution. Yellow powder (3-Indoleglyoxylyl chloride) (3) appears in the beaker.
At the end of the addition of all oxalyl chloride, Rm is stirred for another 10-15 minutes.
(1:59-2:13) - The powder is unstable. If the mixture is coloured red, the product is not suitable for further use. In this case, the process should be repeated, reducing the reaction time
(2:16-2:49) - 3-Indoleglyoxylyl chloride (3) is filtered and washed twice with 50ml MTBE.
(2:50-2:57) - ⚠️ The resulting product hasn't been stored and its contact with air has to be minimized.

STAGE 2/4​

(3:11-3:40) - 3-Indoleglyoxylyl chloride (3) is suspended in 1200ml MTBE under intense stirring and cooling. Next, 40ml of diethylamine is added dropwise to the suspension within 20 minutes. ⚠️ Mixture temperature has to be under 5°C. At temperatures above 5 degrees, the amount of product produced is significantly reduced.
(3:40-4:02) - N,N-diethylindol-3-ylglyoxylamide (4) which was formed in the process is filtered and washed with 50ml MTBE.
(4:02-4:37) - N,N-diethylindol-3-ylglyoxylamide (4) is recrystallized from boiling methanol (25 parts methanol per 1 part amide). ⚠️ The mixture is maintained at -15°C. If crystallization does not begin, dilute Rm with three volumes of ether and leave again for cooling.
N,N-diethylindol-3-ylglyoxylamide (4) is filtered, washed with ether to give, after air drying, 38.8g. Next, in the video, we used half of the resulting powder (19g).

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STAGE 3/4​

⚠️ Be careful when working with LiAH. All utensils should be completely dry. A drop of water can cause a fire! ⚠️
(4:52-5:03) - 19g LiAH is suspended in 350ml anhydrous dioxane.
(5:04-5:14) - A suspension of 19g of N,N-diethylindol-3-ylglyoxylamide (4) in 350ml of anhydrous dioxane was slowly added to the flask.
(5:19-5:28) - Rm is refluxed for 16-26h.
(5:35-5:40) - Rm is moved to the cup and cooled in an ice water.
(5:41-5:57) - Excess hydride is decomposed by dropwise addition of wet dioxane (10-20ml). The mixture remains until the reaction is complete.
(6:01-6:08) - Now the sludge is filtered on the Schott funnel.
(6:09-6:31) - The slurry is washed with hot dioxane (400ml). Filtered again.
(6:36-6:50) - The filtrate is dried over anhydrous MgSO4 for 15-20 minutes.
(6:53-7:07) - After 15-20 minutes, Rm is filtered from sulfate.
(7:20-7:40) - Solvent distilled off to dryness in a rotary evaporator.

STAGE 4/4​

(7:55-8:13) - The resulting oil was diluted with diethyl ether. Followed by saturated with dry hydrogen chloride HCl (dry gas) to 6pH.
💎 The resulting powder (5) was recrystallized from a mixture of boiling benzene and methanol, filtered, washed with diethyl ether, and dried to a constant weight.
Final yield 14,5g (75%) of N, N-diethyltryptamine hydrochloride (DET) (5).​
⚙️ You can find out more about the gas generator here.
 
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MadHatter

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Great video! I seem to recognize the production value and style from somewhere ;).
Anyway, the MTBE reagent is a bit hard to obtain, is it possible to replace with something less obscure? Or do you have any tip on a good OTC source of it?
 

Novator

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Great video! I seem to recognize the production value and style from somewhere ;).
Anyway, the MTBE reagent is a bit hard to obtain, is it possible to replace with something less obscure? Or do you have any tip on a good OTC source of it?
DocXEt₂O (diethyl ether) - is an equivalent replacement for MTBE.

Proportions:
20g indole + 300ml anhydrous Et₂O
22g oxalyl chloride + 300ml anhydrous Et₂O


this is an amazing video! hope to see more :)
When it's possible, we make video for most popular chem reactions. New videos coming soon 🎬
 
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花谢花开

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Et₂O (diethyl ether) - is an equivalent replacement for MTBE.

Proportions:




When it's possible, we make video for most popular chem reactions. New videos coming soon 🎬
NovatorNice to meet you 1. Hello, I would like to ask, does the reflow for 16-26 hours need to be heated? What is the heating temperature? Thank you. Please reply and thank you. 2 In the thread of making 5-meo-dipt, can methyl tert-butyl ether be used as a solvent? I will always look forward to your reply, otherwise I will not be able to sleep. Please reply so that I can sleep well. Thank you very much. a person who needs help
 

Sony2xl

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Great video awesome!
 

nob0dy

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tutorials like those would amazing if there is many
 

Hank Shrader

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View attachment 4487

✅The technique is suitable for the synthesis of popular tryptamines from TIHKAL. For example, replacing diethylamine on dimethylamine (3:20), you will receive DMT.

⚠️The air temperature in the laboratory should not exceed 10°C.
☣️Exhaust ventilation, respiratory and eye protection.

⚙️
Beakers 1000, 500, 250 and 50ml
Filter Flask 2000ml
Flat-bottomed flask 29/32 2000ml
Reflux condenser 29/32
Drop funnel 500 and 60ml
Glass funnel 100 mm
Schott funnel 60 mm
Buchner funnel 100 mm
Long-probe lab thermometer
Magnetic stirrer
Lab support stand
Rotary evaporator
Hot plate with temperature control
Single stage vacuum pump
Filter paper
Mortar and Pestle
Generator of hydrogen gas (dry hydrogen chloride HCl)
Lab spoon spatula (stainless steel)
Glass stirring rod
Crystallizing dishes 60-200mm
Litmus test paper (pH 0-12)
Syringes 20ml (x4)
🛢️
Indole 20g
Oxalyl chloride 22g
Diethylamine 40ml
MTBE 1800ml
Methanol 750ml
LiAH 19g
Anhydrous dioxane 1200ml
Wet dioxane ~10-20ml
Anhydrous MgSO4 20g
Dry hydrogen chloride HCl (gas)
Benzene 250ml
Diethyl ether 300ml
📑

Stage 1/4

Preparation of 3-Indoleglyoxylyl chloride

20g indole + 240ml MTBE
22g oxalyl chloride + 240ml MTBE

Stage 2/4

Preparation of N,N-diethylindol-3-ylglyoxylamide

3-Indoleglyoxylyl chloride + 1200ml MTBE
Rm + 40ml diethylamine

Stage 3/4

Reductive amination of N,N-diethylindol-3-ylglyoxylamide to N, N-diethyltryptamine via LiAH

19g LiAH + 350ml anhydrous dioxane
19g N,N-diethylindol-3-ylglyoxylamide + 350ml anhydrous dioxane

After 26h used 10-20ml wet dioxane

The filtrate is dried over 20g anhydrous MgSO4

Stage 4/4

Crystallization of N ,N-diethyltryptamine hydrochloride (DET)

Oil (Freebase) + 100ml diethyl ether
View attachment 4523

STAGE 1/4​

(0:53-1:10) - 20g of ground indole (1) dissolves in 240ml MTBE
(1:11-1:20) - 22g oxalyl chloride (2) was dissolves in 240ml MTBE
(1:25-1:50) - The oxalyl chloride solution is placed in a dropping funnel and with vigorous stirring, dropwise, within 30 minutes is added to the indole solution. Yellow powder (3-Indoleglyoxylyl chloride) (3) appears in the beaker.
At the end of the addition of all oxalyl chloride, Rm is stirred for another 10-15 minutes.
(1:59-2:13) - The powder is unstable. If the mixture is coloured red, the product is not suitable for further use. In this case, the process should be repeated, reducing the reaction time
(2:16-2:49) - 3-Indoleglyoxylyl chloride (3) is filtered and washed twice with 50ml MTBE.
(2:50-2:57) - ⚠️ The resulting product hasn't been stored and its contact with air has to be minimized.

STAGE 2/4​

(3:11-3:40) - 3-Indoleglyoxylyl chloride (3) is suspended in 1200ml MTBE under intense stirring and cooling. Next, 40ml of diethylamine is added dropwise to the suspension within 20 minutes. ⚠️ Mixture temperature has to be under 5°C. At temperatures above 5 degrees, the amount of product produced is significantly reduced.
(3:40-4:02) - N,N-diethylindol-3-ylglyoxylamide (4) which was formed in the process is filtered and washed with 50ml MTBE.
(4:02-4:37) - N,N-diethylindol-3-ylglyoxylamide (4) is recrystallized from boiling methanol (25 parts methanol per 1 part amide). ⚠️ The mixture is maintained at -15°C. If crystallization does not begin, dilute Rm with three volumes of ether and leave again for cooling.
N,N-diethylindol-3-ylglyoxylamide (4) is filtered, washed with ether to give, after air drying, 38.8g. Next, in the video, we used half of the resulting powder (19g).

STAGE 3/4​

⚠️ Be careful when working with LiAH. All utensils should be completely dry. A drop of water can cause a fire! ⚠️
(4:52-5:03) - 19g LiAH is suspended in 350ml anhydrous dioxane.
(5:04-5:14) - A suspension of 19g of N,N-diethylindol-3-ylglyoxylamide (4) in 350ml of anhydrous dioxane was slowly added to the flask.
(5:19-5:28) - Rm is refluxed for 16-26h.
(5:35-5:40) - Rm is moved to the cup and cooled in an ice water.
(5:41-5:57) - Excess hydride is decomposed by dropwise addition of wet dioxane (10-20ml). The mixture remains until the reaction is complete.
(6:01-6:08) - Now the sludge is filtered on the Schott funnel.
(6:09-6:31) - The slurry is washed with hot dioxane (400ml). Filtered again.
(6:36-6:50) - The filtrate is dried over anhydrous MgSO4 for 15-20 minutes.
(6:53-7:07) - After 15-20 minutes, Rm is filtered from sulfate.
(7:20-7:40) - Solvent distilled off to dryness in a rotary evaporator.

STAGE 4/4​

(7:55-8:13) - The resulting oil was diluted with diethyl ether. Followed by saturated with dry hydrogen chloride HCl (dry gas) to 6pH.
💎 The resulting powder (5) was recrystallized from a mixture of boiling benzene and methanol, filtered, washed with diethyl ether, and dried to a constant weight.
Final yield 14,5g (75%) of N, N-diethyltryptamine hydrochloride (DET) (5).​
⚙️ You can find out more about the gas generator here.
Novatorso if in my garage there is not temperature under 10° i can't start synthesis?
 

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花谢花开

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You have to use A/C. Correct temperature is significantly important for some substances handling.
G.PattonCan methyl tert-butyl ether be used instead for the final stage of washing?
 

花谢花开

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You have to use A/C. Correct temperature is significantly important for some substances handling.
G.PattonI saw you posted a new tutorial but I am still interested in this. Hello, can I ask one more question? Is it possible to use methyl tert-butyl ether as a solvent when making 5-meo-dipt on this thread? 2. Approximately what temperature does the reflow need to be heated to for 16 to 26 hours?
 

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I saw you posted a new tutorial but I am still interested in this. Hello, can I ask one more question? Is it possible to use methyl tert-butyl ether as a solvent when making 5-meo-dipt on this thread? 2. Approximately what temperature does the reflow need to be heated to for 16 to 26 hours?
花谢花开Hello again. Thanks for kind words. As I said, I cannot say for sure concerning methyl tert-butyl ether as a solvent, I guess it will be not so good idea. You can carry out an experiment in a small scale.
So far as temperature concerned, it is temperature, when the mixture is boiled (mostly depends on a used solvent boiling point).
 

Whatnowtodowhen

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Does anyone know of any decent acacias in tasmania worth harvesting?
 

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Hello. In the internet I found a lot of synthesis from tryptophan to tryptamine and from tryptamine to basically everything. Tryptamine to dmt needs sodium cyanobrohodydride, which is expensive. Is there any way doing it with a cheaper reduction agent? And if yes, how?
 

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Hello. In the internet I found a lot of synthesis from tryptophan to tryptamine and from tryptamine to basically everything. Tryptamine to dmt needs sodium cyanobrohodydride, which is expensive. Is there any way doing it with a cheaper reduction agent? And if yes, how?
BlackyHi. Have you seen this video and read topic? You can do if from indole.
 

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beautiful in every sense since it encourages me not to fear the bisindole byproduct that I thought would form by mistake... if say my desired final product is MIPT the amine is pretty expensive... would the route starting from tryptamine and then acetone imine/reduction followed by formaldehyde methylimine and another reduction be more cost effective? (DIPT is undesired)
 

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Can I replace the indole in this process with 4-aco indole to make 4-aco dmt?
 

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Your assumption is absolutely correct and the answer is yes. The fact taht you had to ask betrays the fact that you will most probably end up with gunk first 2-3 tries so keep it all downscale nothing above 0,1g. The prep has some difficulty associated so you need practical experience or some development I can provide and then do as I tell you. I myself am not lucky enough to have 4AcO-indole around. Sourcing Oxalyl chloride in EU i know how to do, as well as LAH. Note that oxalyl chloride is a diacyl chloride therefore it has two business ends that can react with indole (this alone shoud make you a good idea why is unadvised to be insufficiently prepared). Cheers!
 

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Would using 5-meo-indole work in place of indole to make 5-meo variants?
 

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