Novator

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✅This method is suitable for the synthesis of Mescaline and its analogues (look Pihkal).

☣️Exhaust ventilation, respiratory and eye protection are needed.

⚙️
  • Beakers 25, 50, 100 (x2), 250 и 500 mL
  • Reflux condenser 29/32
  • Lab support stand
  • Hot plate with temperature control
  • Magnetic stirrer
  • Flat-bottomed flask 29/32 1000, 2000 mL
  • Rotary evaporator
  • Glass funnel d=100 mm
  • Single stage vacuum pump
  • Drop funnel 500 and 60 mL
  • Litmus test paper (pH 0-12)
  • Glass stirring rod
  • Bunsen flask 500, 2000 mL
  • Buchner funnel d=100 mm
  • Filter paper
  • Generator of hydrogen gas (dry hydrogen chloride HCl)
  • Lab spoon spatula (stainless steel)
  • Syringes 20ml (x2)
  • Mortar and Pestle
🛢️
  • 3,4,5-trimethoxybenzaldehyde 20g (cas 86-81-7)
  • Nitromethane 100ml (for Mescaline synthesis) or Nitroethane 80ml (for TMA synthesis)
  • Anhydrous ammonium acetate (AcONH4) 5g
  • Methanol 100ml
  • IPA 500ml
  • THF 350ml
  • LiAH 10g
  • NaOH 7.5g
  • Ethyl acetate 150ml
  • Dry hydrogen chloride HCl (gas)
📑

Stage 1/3

Preparation of 3,4,5-trimethoxy-nitrostyrene (for Mescaline) or 3,4,5-trimethoxy-nitropropene (for TMA)
by condensation from 3,4,5-trimethoxybenzaldehyde


20g 3,4,5-trimethoxybenzaldehyde + 100ml Nitromethane (for Mescaline) or 80ml Nitroethane (for TMA)
+ 5g Anhydrous ammonium acetate (AcONH4)

Stage 2/3

Reductive amination of 3,4,5-trimethoxy-nitrostyrene/propene
to Mescaline/TMA via LiAH


THF (50ml per 10g) + 3,4,5-trimethoxy-nitrostyrene/propene
250ml THF + 10g LiAH

25ml H₂O
7.5g NaOH

Stage 3/3

Preparation of Mescaline or TMA hydrochloride salts

Oil (Freebase) + 150ml Ethyl acetate
Stage 1/3 (00:00-03:07)
⚠️The condensation reaction is typical and suitable for the preparation of 1-(2,5-dimethoxyphenyl)-2-nitropropene which is intermediate for the synthesis of a such psychedelic as 2,5-dimethoxy-4-bromoamphetamine (DOB).

20 g of 3,4,5-trimethoxybenzaldehyde is added to the flask 100 mL Nitromethane (for Mescaline) or 80ml Nitroethane (for TMA)
5g Anhydrous ammonium acetate (AcONH4)
Rm is stirred with a magnetic stirrer for 10 minutes
Then Rm is boiled in the round bottom flask (1000ml) with attached reflux condenser for 1-2 hours
⚠️ The solution is boiled until a deep orange color is reached. ⚠️

Then Nitromethane (Nitroethane for TMA synthesis) without residue is distilled off in a rotary evaporator
⚠️ Remember that special hoses have to be used for a vacuum handling. Also, the trap is practically useless in this case.
⚠️ The nitromethane which was collected in the receiving flask is suitable for further use.

3,4,5-Trimethoxy-nitrostyrene (for Mescaline synthesis) or 3,4,5-Trimethoxy-nitropropene (for TMA synthesis) remain in the flask
They crystallize during cooling
⚠️ The solution is placed in the freezer. The product crystallize as spectacular crystal needles.

The resulting styrene (or propene) is recrystallized by methanol in a ratio of 1:10
Crystals are filtered and washed with cooled IPA
⚠️ Do not neglect additional purification at each of the synthesis steps. The purity of the benzaldehyde condensation product significantly affects the quality of the final result.
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Stage 2/3 (03:08-09:37)
THF (50ml per 10g) was added to 3,4,5-trimethoxy-nitrostyrene
Stir the solution until the substance is completely dissolved
Rm is poured into the drip funnel

In a flat-bottom flask (2000 mL), 10g of LiAH is gradually poured with 250ml of THF
(optimal use of a two-necked flask)
⚠️ All reagents and glassware must be absolutely dry. The reaction in the presence of water is unacceptable. A safety violation can cause the mixture to ignite.

Flask immersed into ice water, supplied with reflux condenser and drip funnel
Through reflux condenser, the benzaldehyde condensation product, which was dissolved in THF, is added dropwise to Rm
⚠️ The reaction is exothermic!
Funnel and reflux condenser are washed with a small amount of THF
Rm
is then boiled with attached reflux condenser for 2-4 hours

After a while, the flask is cooled by ice water
Distilled water is slowly added dropwise and the LAH exess are decomposed
⚠️ It worth to start with 10 ml of distilled water, and than add a NaOH solution (about 15 ml).
Rm pH is corrected with NaOH solution to 11pH
⚠️ pH measurements are carried out using a glass rod. The glass rod is immersed in the solution and then this glass rod with drop of the solution is touched an indicator paper.
Rm have to be stirred for 10 minutes

Then, the solution have to stay without stirring for one hour until layers are separated
⚠️ Some chemists leave the solution to stay for 24 hours.

Rm is filtered through paper filter
Vacuum release by a ball valve will significantly extend the life of the pump

After filtration, THF is completely distilled off from the solution
⚠️ The evaporation of the solvent is carried out in batches or at one time, it is depends on the volume of the rotary evaporator flask.
If condensate is no longer visible in the reflux condenser of the rotary evaporator, it means that all THF was evaporated
⚠️ The resulting free base can be distilled in a high vacuum for absolutely purity level of the product.

Free base (TMA or Mescaline) is dissolved in a portion of ethyl acetate
⚠️ The solution have to be dried over the dehydrated MgSO4 (approximately 10 minutes), if a visible water particles are there.
The solution is placed on a magnetic stirrer
⚠️ Rm have to be cooled and shouldn't be heated during acid is addition.
Simz2xuIQH

Stage 3/3 (09:38-11:53)
Mescaline can be crystallized with sulfuric acid, but Mescaline sulfate has a higher dosage
Therefore, gas generator of dry hydrogen chloride gas should be used for Mescaline and TMA
e.g. from sodium chloride and sulfuric acid
The most convenient solution is the using of dioxane hydrochloride
⚠️ Dioxane hydrochloride, unlike hydrochloric acid, does not contain water

Rm pH is adjusted to 6pH
If the mixture is too thick, it is possible to dilute with a portion of ethyl acetate
The solution exactly equal to 6pH
Rm
should now be kept in the freezer for one hour

The final product is filtered
The final product have to be washed with cooled IPA
⚠️ If you suspend the hydrochloride in a portion of IPA and filter the suspension again, the powder would completely white.

💎 The final yield of mescaline hydrochloride is not less than 19g. 💎

⚙️ You can find out more about the gas generator here.
 
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diogenes

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Where can 3,4,5 trimetoxybenzaldehyde be bought? Or is there a way to synthesize this? I haven`t found anything in the forum. Any advice would be appreciated. The rest of the starting materials are relatively easy to get.
 

Ihatemybitchwife

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diogenes

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Thank you Ihatemybitchwife. It looks to me that the best/easiest way is the route to start from Vanillin especially because it is readily available. Can someone more experienced confirm/deniy this?
 

Sneaky.Base

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Hi everyone. I have a silly question about tma 2.
There are 2 ways to synthesis tma2 from 2.4.5m:

calmus oil --> Arasone --> 2,4,5-trimethoxy-benzaldehyde --> 2,4,5-trimethoxy-phenyl-2-nitropropene --> TMA-2

And

arasone --> 2,4,5-Trimethoxyphenyl-2-nitropropene --> 2,4,5-Trimethoxyphenyl-2-propanone --> TMA-2

Right?

As Asarone is 2,4,5-Trimethoxyphenyl-2-propene why not turn it into 2,4,5-Trimethoxyphenyl-2-nitropropene then reduce to tma2? Just 2 step
You dont even need fucking nitroethane .
As my question is silly im greatfull if sombody explain my mistake. Tnx
 

G.Patton

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Hi everyone. I have a silly question about tma 2.
There are 2 ways to synthesis tma2 from 2.4.5m:

calmus oil --> Arasone --> 2,4,5-trimethoxy-benzaldehyde --> 2,4,5-trimethoxy-phenyl-2-nitropropene --> TMA-2

And

arasone --> 2,4,5-Trimethoxyphenyl-2-nitropropene --> 2,4,5-Trimethoxyphenyl-2-propanone --> TMA-2

Right?

As Asarone is 2,4,5-Trimethoxyphenyl-2-propene why not turn it into 2,4,5-Trimethoxyphenyl-2-nitropropene then reduce to tma2? Just 2 step
You dont even need fucking nitroethane .
As my question is silly im greatfull if sombody explain my mistake. Tnx
Sneaky.BaseHi, I think it is possible.
As Asarone is 2,4,5-Trimethoxyphenyl-2-propene why not turn it into 2,4,5-Trimethoxyphenyl-2-nitropropene then reduce to tma2? Just 2 step
You dont even need fucking nitroethane .
 

Sneaky.Base

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If you think its possible as a professional. It is worth trying once
 

FunkyDude3000

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can a vacuum distillation can be used here instead of the rotovap to remove and collect the nitromethane/ethane?
 

Phi

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Can anyone advise if a NaBH4 reduction in methanol would substitute for the LiAH?
 

Phi

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Can anyone advise if a NaBH4 reduction in methanol would substitute for the LiAH?
PhiAnswered my own question for anyone else who's interested

 

amieri

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General P I need you buddy.whats some ways around the Lah,or is it possible to make?
 

PsychedelicDog

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@Novator hi how much Dioxane hydrochloride is to be used here? And what product is used to adjust the ph?
 

G.Patton

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@Novator hi how much Dioxane hydrochloride is to be used here? And what product is used to adjust the ph?
PsychedelicDogDioxane hydrochloride is solution of HCl acid in dioxane (solvent). You can use this solution to adjust pH 6. Amount of this solution depends of you synthesis scale and its concentration.
 
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