WillD

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Reagents:
M4

  • 3,4,5-Trimethoxybenzaldehyde (cas 86-81-7) 1000 g;
  • Acetic acid 5 L;
  • Nitromethane (cas 75-52-5) 2 L;
  • Cyclohexylamine (cas 108-91-8) 100 ml;
  • Distilled water ~17 L;
  • Isopropyl alcohol (IPA) ~23 L;
  • Sodium borohydride (NaBH4) 1200 g;
  • Copper chloride (CuCl2) 72 g;
  • Sodium hydroxide (NaOH) 25% aq. 8 L;
  • Magnesium sulfate (MgSO4);
  • Acetone 2.5 L;
  • Sulfuric acid (H2SO4 conc.) ~410 mL or hydrochloric acid (HCl conc.) ~150 mL;
Equipment and glassware:
Step 1. Beta-nitro-3,4,5-trimethoxystyrene synthesis (cas 6316-70-7) from 3,4,5-trimethoxybenzaldehyde.
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1. 3,4,5-Trimethoxybenzaldehyde (cas 86-81-7) 1000 g , acetic acid 5 L and nitromethane 2 L are added into a 20 l flask.
2. The reaction mixture is stirred and cyclohexylamine 100 ml is added.
3. The mixture is heated to 80 °C and stirred for 3 h.
4. Distilled water 10 L is added dropwise with constant stirring. Yellow crystals are formed.
5. Crystals are
filtered and washed with distilled water.
6. Then, they are air dried at room temperature.
7. Next, crystals are dissolved in boiling hot IPA (
as minimum as possible) and put into a freezer for 12 h.
8. Crystals are
filtered, washed with a small amount of cold IPA and air dried after the solution crystallization procedure 7. Beta-nitro-3,4,5-trimethoxystyrene (cas 6316-70-7) yield is 920 g.

Step 2. Beta-nitro-3,4,5-trimethoxystyrene reduction with NaBH4/CuCl2 to mescaline.
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1. Isopropanole-water mixture (IPA/H2O 2:1) 18 L is added to a 50 L batch reactor.
2. Sodium borohydride (NaBH4) 1200 g is added in one portion at a constant stirring.
3. Beta-nitro-3,4,5-trimethoxystyrene (cas 6316-70-7) 1000 g is added in small portions so that the mixture temperature is kept below 60 °C.
4. Copper chloride (CuCl2) 72 g in distilled water 200 ml is added dropwise so that the mixture temperature is kept below 80 °C.
5. Thereafter, the reaction mixture is held at 80 °C for 30 min with help of an external heating.
6. Sodium hydroxide 25% water solution (NaOH) 8 L is added to the reaction mixture, mixed well. Obtained layers are separated.
7. The aqueous layer is
extracted with IPA 8 L (or DCM, or ether, or benzene). Extracts are combined and dried over magnesium sulphate (MgSO4).
8. Solvent is
distilled off under reduced pressure to an oil.
9. The oil is dissolved in dry acetone 2 L.
10. Sulfuric acid (H2SO4 conc.) or hydrochloric acid (HCl conc.) is added dropwise with a constant stirring to reach pH 6.
11. The mixture is put into the freezer for 12 h.
12. The suspension is
filtered and washed with a dry cold acetone after crystallization procedure. Mescaline (cas 642-73-9 or cas 832-92-8) yield is 60-70%.
M2
 
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Octopusssss

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Hello
The synthesis can be more simple and it also works with smaller scale

To make it more simple we can change this points from step 2:

7. The aqueous phase was extracted with 8 liters IPA, DCM, ether or benzene.

Let the layesr separate - leave it for some time. Take uper layer. Whats left can be extracted by ading IPA. Than we can put uper layer and IPA from washing together.

8. We will add 30% H2SO4 to the yellow liquid from point 7. We do it drop by drop with stiring that the PH will go to PH 6. Drop by drop slowly. Than we can see that this starts to be milky and we can see cristals. We can leave it in fridge (i dont know if this will help) and than we filter it.

9. We are left with mescaline sulftae dihydrate. Its nice white and we can wash it with aceton in we want. Its (C11H17NO3)2 x H2SO4 x 2H2O

This make easy - we dont need vacum...
 

G.Patton

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>>This make easy - we dont need vacum...

Probably it will works with a very small scale. I'm sure that your product will not crystallize in 8 L of solvent. By this reason, you have to evaporate solvent. Also, acetone from step 9 pull out water and accelerates crystallization.
 
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Octopusssss

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I try this in 10g nitrostyren - i scale all reaction from second part and i get from starting 10 gram of nitrostyrene and the efect is 4,5 gram of mescaline sulfate.
 

Mr Gonzo

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Hi with regards to the LAH is there something else thats is more easy to obtain and use in its place, or is there some way I could be instructed on how to buy the hydride from somewhere with minimal hassle? Tried a place in India and they was having none of if! I'm based in UK
 

FredDurst

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Hi with regards to the LAH is there something else thats is more easy to obtain and use in its place, or is there some way I could be instructed on how to buy the hydride from somewhere with minimal hassle? Tried a place in India and they was having none of if! I'm based in UK
Mr GonzoDid you source some for the UK in the end mate?
 

BufoKing

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Did you source some for the UK in the end mate?
FredDursti got 100g of LAH i’m no longer using. it’s unopened in a soup can. if you want it, i’ll give ya a good price.
i just sodium borohydride /cucl2 for everything i was gonna use it for.
 

FredDurst

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i got 100g of LAH i’m no longer using. it’s unopened in a soup can. if you want it, i’ll give ya a good price.
i just sodium borohydride /cucl2 for everything i was gonna use it for.
BufoKingIll inbox you mate
 

HerrHaber

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You may try NaBH4/CuCl2 method if LAH is too scary for you, or you are newer to preparative chemistry. LAH can spontaneously ignite if miss-handled or kept in ambient for long enough.
 

amieri

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Scaling this down could you drop all of the reagents down by say a tenth or would a person need to do molecular equivalency? that's still very new to me any suggestions on how to do it or where to learn it? thanks in advance
 

WillD

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Scaling this down could you drop all of the reagents down by say a tenth or would a person need to do molecular equivalency? that's still very new to me any suggestions on how to do it or where to learn it? thanks in advance
amierifor large scale u can go via 3,4,5-trimeophenylacetone
 

amieri

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Finding 345-tmba isn't horrible hard and nitromethane seems possible to make from some YouTube videos but not with the greatest of yeids.how would one go about trying this with 10 grams of tmba? Would you just divide everything down?if anyone can help point someone in the right direction I'm sure they'd appreciate it alot.
 

WillD

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Finding 345-tmba isn't horrible hard and nitromethane seems possible to make from some YouTube videos but not with the greatest of yeids.how would one go about trying this with 10 grams of tmba? Would you just divide everything down?if anyone can help point someone in the right direction I'm sure they'd appreciate it alot.
amieriYou can use chloropropionate with this aldehyde to get phenylacetone via glycidate. If this reagent is easier for you than nitromethane, which is regulated.
 

amieri

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Would the reagents list look like this?
100g tmba
.5l acetic acid
.2l nitromethane
10ml cyclohexane
1.7l distilled water
120g NaBH4
7.2g cuCl
0.8l NaOH
.25l acetone
41ml H2so4
Or are there molecular equivalencys I need to take into consideration
 

faszom

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Hello.
If I change nitromethane to nitroethane, can I make tma using this nabh4 method?
 

amieri

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Hello.
If I change nitromethane to nitroethane, can I make tma using this nabh4 method?
faszomAwesome question I've been searching for the answer too.u believe so but hopefully someone experienced will join in
 

plancklong

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A glaring problem that I see is that IPA and water are completely miscible. How are you even going to get layerS! Does this alarm, or even concern anyone else?

Has anyone actually done this synthesis as written?

If I am missing something, please let me know!
 

Swirly

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A glaring problem that I see is that IPA and water are completely miscible. How are you even going to get layerS! Does this alarm, or even concern anyone else?

Has anyone actually done this synthesis as written?

If I am missing something, please let me know!
plancklongI have not done this synthesis but when making 2c-b using a very similar method the water layer falls to the bottom once it picks up sodium borohydride. Likewise water and IPA separate when one holds the freebase.

IPA and water are completely miscible BUT they will form layers IN CERTAIN CONDITIONS. And the layers will be very distinct. You can actually use fresh IPA to pick up whatever the aqueous layer has and they will not mix.
 

Muktika

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Is it possible to get a smaller volume in step 1 by reducing all ingredients by 10 times?
 
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