# Mescaline and TMA synthesis (and analogues). Video manual.



## Novator (Jul 31, 2022)

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Mescaline and TMA synthesis (and analogues). Video manual.



__ Novator
__ Aug 1, 2022
__ 5
__
cas 1082-88-8
cas 54-04-6
cas 86-81-7
mescaline video
peyote
synthesis
tma video
tmpea
trimethoxyamphetamine
video manual




This method is suitable for the syntheses of Mescaline and its analogues...







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

Exhaust ventilation, respiratory and eye protection are needed.



Spoiler: Equipment and glassware





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






Spoiler: Reagents





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)






Spoiler: Chemical proportions




*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





Spoiler: Synthesis



*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.


*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.


*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

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.


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## Ihatemybitchwife

diogenes said:


> 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.



diogenes





Explore 3,4,5-Trimethoxybenzaldehyde | ShulginIndex · info


Explore the structures and analogues of 3,4,5-Trimethoxybenzaldehyde, 3,4,5-TMBAL in book II of The Shulgin Index, Volume One: Psychedelic Phenethylamines and Related Compounds. Alexander T. Shulgin, Tania Manning and Paul F. Daley.



isomerdesign.com


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## diogenes

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?


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