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 chloride20g indole + 240ml MTBE
22g oxalyl chloride + 240ml MTBE
Stage 2/4
Preparation of N,N-diethylindol-3-ylglyoxylamide3-Indoleglyoxylyl chloride + 1200ml MTBE
Rm + 40ml diethylamine
Stage 3/4
Reductive amination of N,N-diethylindol-3-ylglyoxylamide to N, N-diethyltryptamine via LiAH19g 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
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.
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