Mescaline Synthesis With Nitromethane. 1000g Scale.

[Mr Gonzo]

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]

Did you source some for the UK in the end mate?

 

[Rabidreject]

lol I did the exact same thing! I’m pretty scared to go near the LAH!

 

[Rabidreject]

Does the second bit of this synth work nicely scaled down to say a 5g starting nitrostyrene quantity? Or do the solvents scale differently? I’m about to try this…

 

[Rabidreject]

Oh one more thing, can I reduce the corresponding nitropropene for TMA in the same manner? It seeems okay but it would comfort me to know someone has done it!

 

[Rabidreject]

This is bugging me - I’m about to perform your reaction and have scaled everything down but I still find myself wondering this…

Why do you say to add the b-3,4,5-TMONS in portions as a powder, as opposed to dissolving it and adding dropwise?

Is it a scale thing that I’m missing because I have never worked on a scale even close to this?

 

[Swirly]

Dump in the nitrostyrene about 3 large spoonfuls at a time under crushed ice-salt-bit of water cooling. The sodium borohydride/IPA/h20 should be cooled to about 5 -8 celcius when you begin the nitrostyrene addition, as when you add a larger amount of nitrostyrene it does heat up some.

If you pour everything in at once it will be a runaway volcano, crazy action, too much heat.

Keep it under 26 - 28 C. Depending on the nitrostyrene and amount, addition might take over an hour. You will need to add more ice if taking a long time and working with lets say 100g.

If yours is a small amount, might be able to dump everything in at once without temp. spiking too much.

 

[Rabidreject]

Yeah I’m literally just testing on a 5g scale at the moment.

Iv been learning and due to the fact there is such a difference in the amount being added, I’m assuming I didn’t reflux it long enough.

I think I was expecting it to be way more exothermic than it was, due to the fact I did such a small scale reaction and therefore it was quite a bit cooler than the synth said upon addition. I don’t think I let it react for long enough at around 75c.

Im surprised by your temps to be honest but I guess as you say it differs depending on which styrene you are using? I dunno…it’s strange that it didn’t look like the organic solvent extracted anything out of the aqueous phase tbh.

 

[Swirly]

Yes, 2,5-DMNS seemed to give off less heat and did not react as vigorously as 3,4,5-TMNS at the same amounts. I was able to add the DMNS quicker and it fully dissolved, i.e. no orange/yellow was left. While I could not get the reaction mixture to go fully milky white with 3,4,5-TMNS, always a touch of yellow left.

I read elsewhere that temps are kept below 30 C during addition. Someone wrote that it increases yield or something. This was for 2,5-DMNS I believe, so I do this for 3,4,5-TMNS as well. Keep it all under the ice.

 

[Rabidreject]

Ahhh okay I get you.
That all makes sense…

Honestly, I used my first lot of the 3,4,5-NS in the first reaction and didn’t get squat out of it (5g scale). Not exactly sure where I went wrong but it certainly didn’t get too hot but I also didn’t let it react for very long at all….I just know when I went to extract the aqueous layer with DCM there was next to nothing in it…

Oh well, I often f up first go…so we’ll see but I also had to knock up more of the nitrostyrene as I can get more NM where as NE is more expensive and the 2,5- aldehyde I have less of as it’s more expensive compared to 3,4,5.

Oh I’m also going to write everything I do in the next reduction down lol