I never tried this one, but here are a few thought:
Your starting chemicals are not a problem (just hope you didnt bought them at same source
![Wink ;)](https://thevespiary.org/talk/Smileys/default/wink.gif)
)
He washed the yellow - orange oil with dH2O to remove any acid/base, dissolved it in MeOH, EtOH or IPA and filtered it with a drying agent to remove any water traces.Plain water can be used instead of dH2O, it's cheaper... And you cannot dry a compound when it is dissolved in an alcohol, the alcohol will most likely react with the drying agent.
Then he put the samples in the freezer and looked at it from time to time, but even after two days in the freezer ( -18°C ) no crystals were produced. So he decided to eject this reaction.Well next time dont throw it away, put it in a rbf, big enough to do a good evaporation, then distill of the alcohol in vacuum, see if you have crystal or oil remaining. Then try to work with the oil to see if it crystallise or not. Once you have crystal, continue the workup by dissolving them and putting in freezer or whatever.
But at day 14 no more water was produced and the color changed to a very deep orange. He knows this is a sight of decomposition, but he tried to crystalize it like before - with and without solvent - but no results.Well the deep orange is not always a sign of decomposition, here i think it is your solvent getting more and more charged with nitropropene (and this is a good thing
![Smiley :)](https://thevespiary.org/talk/Smileys/default/smiley.gif)
).
1 mole Benzaldehyde, 1.1 mole Nitroethane and 0.1 mole n-butylamine were mixed in a flask and the air was pumped out with vacuum to prevent decomposition while reacting. The flask was put in a warm water bath ( 40 - 50°C ) for about 2 hours.....Here i am afraid that at 40-50° with a vacuum you are evaporating your catalyst... Better make the acetate and dont use a vacuum, air will not bee that bad for those compounds at that temperature.
Hell stop to think all decompose so fast too
![Grin ;D](https://thevespiary.org/talk/Smileys/default/grin.gif)
if your reaction even turn red it is good, your product is colored, dont forget. BTW you dont use any solvents in that reaction?
Well you should also try to put your benzaldehyde (20g), and nitroethane (20mL) + some catalyst (ammonium acetate or butylammonium acetate)(1-2g) in the MW oven, with a glass of cold water near, and nuke that on defrost for a few minutes (repeat the cycle 2 or 3 times, and let cool down a few minutes between the cycles too), it could work. Then evap the nitroethane off, in vacuuo, and recrystallise the oil/crystals with an appropriate solvent i dont know
![Tongue :P](https://thevespiary.org/talk/Smileys/default/tongue.gif)
. Post result back here after.
Good luck