Okay so I don’t have a rotovap and the synthesis said to remove the excess solvent under vacuum and so the only option I really have atm was just a normal vacuum distillation.
So I set it up using my mantle and rotary vane pump.
Im left with a dark amber/ red oil (I imagine also some residual nitromethane). I shall try to make it crystallise with temperature modifications but if it refuses to grow any crystals I guess ill have to re-x the oil from something - this is the TMA Henry reaction I am trying here as I had good success with the nitrostyrene version of the same reaction.
As I said, I essentially followed the video on here for mescaline/TMA whilst also reading Shulgin’s write-up’s as he mentions things like colour etc. I think he may have been left with an oil in this synth as well but honestly iv read so many different Henry reactions in the past few weeks I think my head is a little overloaded with such similar stuff.
I should really just try a synthesis from start to finish but I never seem to manage that!
I realised earlier that I already have two nitrostyrene’s to reduce - if this TMA synth does work for me and I get crystallisation of the nitropropene then when I come to reduce them all, I’m going to have lots of things to try…bit of a silly way of doing things really but hey ho!
Oh also I weighed the dry, crude b-3,4,5-TMONS and I think it was around 8g.
I know that probably seems really inaccurate and an estimate and to some degree it is coz I weighed it this morning…I dropped again on my meds a couple days ago so my heads pretty foggy.
Anyway thanks for all the help and suggestions - I’m going to start trundling onwards with the reductions now I think.
I have essentially been waiting for around 20-25 years to try mescaline and first bought a mescaline producing cactus around then. I now have so many huge different Trichocerius species - I don’t much fancy chopping up 20+ year old, beautiful cacti when you can just order an aldehyde from bloody china!
Also from my understanding a lot of the sickness with mescaline comes from the plant matter people don’t get rid of properly or just eat the cactus flesh itself.
Either way, I’m a big baby about feeling sick so iv never gotten round to it…
Now I am just one step away - okay well, two or three depending on how much re-x’ing I have to do.
It would be nice to have that one nitropropene though; I must admit.
I seem to have issues making nitropropene’s so I’m guessing the nitroethane I can obtain, isn’t as good or pure after distillation as the nitromethane mix I buy.
I really would like a rotovap, I must admit.
I was surprised how high I had to put my mantle just now when I was doing a vacuum distillation.
The vacuum was held at 0.9 bar, temperature was 40c on the distillation thermometer and just above that on the one in the actual RM.
I was just surprised at how high I had to have my mantle, even though the temperature was low inside the flask.
That was the first vacuum distillation I have done and I shut it off just as it was getting close to 70c purely because the guy in the synthesis set his rotovap bath to 82 and so I figured I didn’t want to heat it too much…
It really annoys me when I see people who use a rotovap to extract things to use in their ‘mixology’ making alcoholic drinks.
I see people like that on YouTube and although I appreciate using tools for things they aren’t really made for, I’m not ashamed to admit I’m just jealous of them!
I know people say you don’t need one unless you have a certain amount of output but still, it would cut down on ordering solvents - which is fairly important for a ‘clandestine’ lab. (Not that I’d really call my place a lab but I guess it is in a loose sense of the word!)
Certainly in the sense of things like DCM, which I’m not really allowed - it just cuts down on danger.
Honestly though I think I’d use one for reducing reaction mixtures and re-x’s. Getting things to crash out without being exposed to a load of air. Vacuum distillations are a bit of an ass compared to simple pouring whatever you have into a flask and switching a device on!
