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- Dec 2, 2023
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Okay, so I tried the nitroaldol reaction using ethanol as the solvent as I don’t have huge amounts of nitromethane to use as solvent as well.
I stupidly refluxed for only two hours, not realising that the shulgin method from which the guy whose video I was watching took it from, was also using NM as the solvent, using ammonium acetate? From what I can remember.
Anyway long story sort of short, I can’t get it to crystallise - which is leading me to think the reaction didn’t run to completion given that styrene’s are meant to be super easy to X’stalise…
I only have a shit hotplate - the cheap one that almost everyone buys from china (SM2 or someshit - iv seen it under different brands but the front panel is either blue or red and it’s like 10cmx10cm) sort of all beyond the point and honestly I dunno if it would even go up to 101c, probably tbf but either way that wasn’t the issue here,
I only refluxed for two hours and then just stirred at RT all night but as I say, when poured over ICY ICY COLD isopropyl, it didn’t crash out. It’s currently in the freezer but clearly something isn’t right as everyone always mentions how easy it is to crystallise these bad boy molecules!
I guess the reason I mentioned my hot plate is I just bought a new heating mantle because when I bought mine, I was so enamoured by the digital temp display that I forgot to actually check it had a friggin’ mag stirrer! It was a serious![Face with rolling eyes :rolling_eyes: 🙄](https://cdn.jsdelivr.net/joypixels/assets/6.5/png/unicode/64/1f644.png)
annoying situation.
To be fair, i actually haven’t needed a mantle with a stir bar until now as I have only done cold, reductive amination of tryptamine into various psychoactive ones.
I have been sort of trying to move onto the nitroaldol reaction with 2,5-TMOBA or 3,4,5-TMOBA, in order to make my own phenethylamines as well…
I particularly wanted to mess around with the ‘scaline compounds as iv never tried any…
It may be a little overload for this thread but I will admit I tried some TLC for the first time yesterday.
I made a mix of 8:2 ethyl acetate: methanol and used it for my mobile phase.
I got a plate (only realised a couple of things after I had actually done it, like holding the plates by the edges like an old school photograph) but I also probably didn’t ‘spot’ small enough as I just used a capillary tube without holding a torch to the middle and pulling to make a micro pipette or whatever they are called…
Oh yeah shit I also left it in the developing tank for too long, didn’t realise you were supposed to pull It out before it covers the whole plate…
So I am aware that I need to practice my TLC before trying…really anything, again tbf…
So I guess after all of that, it’s a bit of a stab in the dark asking you guys why it’s not crystallising!!
One thing I love about organic chem is the catch 22 of needing a seed crystal of a substance that won’t crystallise, in order to get it to crystallise…lol
I stupidly refluxed for only two hours, not realising that the shulgin method from which the guy whose video I was watching took it from, was also using NM as the solvent, using ammonium acetate? From what I can remember.
Anyway long story sort of short, I can’t get it to crystallise - which is leading me to think the reaction didn’t run to completion given that styrene’s are meant to be super easy to X’stalise…
I only have a shit hotplate - the cheap one that almost everyone buys from china (SM2 or someshit - iv seen it under different brands but the front panel is either blue or red and it’s like 10cmx10cm) sort of all beyond the point and honestly I dunno if it would even go up to 101c, probably tbf but either way that wasn’t the issue here,
I only refluxed for two hours and then just stirred at RT all night but as I say, when poured over ICY ICY COLD isopropyl, it didn’t crash out. It’s currently in the freezer but clearly something isn’t right as everyone always mentions how easy it is to crystallise these bad boy molecules!
I guess the reason I mentioned my hot plate is I just bought a new heating mantle because when I bought mine, I was so enamoured by the digital temp display that I forgot to actually check it had a friggin’ mag stirrer! It was a serious
![Face with rolling eyes :rolling_eyes: 🙄](https://cdn.jsdelivr.net/joypixels/assets/6.5/png/unicode/64/1f644.png)
![Weary face :weary: 😩](https://cdn.jsdelivr.net/joypixels/assets/6.5/png/unicode/64/1f629.png)
To be fair, i actually haven’t needed a mantle with a stir bar until now as I have only done cold, reductive amination of tryptamine into various psychoactive ones.
I have been sort of trying to move onto the nitroaldol reaction with 2,5-TMOBA or 3,4,5-TMOBA, in order to make my own phenethylamines as well…
I particularly wanted to mess around with the ‘scaline compounds as iv never tried any…
It may be a little overload for this thread but I will admit I tried some TLC for the first time yesterday.
I made a mix of 8:2 ethyl acetate: methanol and used it for my mobile phase.
I got a plate (only realised a couple of things after I had actually done it, like holding the plates by the edges like an old school photograph) but I also probably didn’t ‘spot’ small enough as I just used a capillary tube without holding a torch to the middle and pulling to make a micro pipette or whatever they are called…
Oh yeah shit I also left it in the developing tank for too long, didn’t realise you were supposed to pull It out before it covers the whole plate…
So I am aware that I need to practice my TLC before trying…really anything, again tbf…
So I guess after all of that, it’s a bit of a stab in the dark asking you guys why it’s not crystallising!!
One thing I love about organic chem is the catch 22 of needing a seed crystal of a substance that won’t crystallise, in order to get it to crystallise…lol