1-Phenyl-2-nitropropene (P2NP) Video Synthesis From Benzaldehyde and Nitroethane. Henry Reaction.
- Thread starter GhostChemist
- Start date
When using aqueous acetic acid, you will most likely have to use some alcohol all at once to dissolve the water, benzaldehyde, and nitroethane together.
like 100 ml benzaldehyde, 100 ml nitroethane, 20 ml acetic acid 80%, 5ml isopropanol and 10ml (or 20ml?) cyclohexilamine in 1 L flask and reflux ?
Last edited:
Mix everything and add isopropanol until the mixture becomes homogeneous. After add a little more for boils and start the reaction.
i have tried ! and it's my actual yield record haha thanks !!
55gr benzaldehyde
40gr nitroethane
10ml acid acetic 80°
3ml isopropanol 99.9%
10ml cyclohexylamine
2:20 p.m. - start of mixing, hotplate at maximum
2:28 p.m. - seems homogeneous to me, with small oily reflections but if I don't see any bubbles
2:32 p.m. - I see bubbles forming in the liquid
2:33 p.m. - I lower the temperature (as I usually do) and turn on the mixer, strong for a few minutes then reduce it a little
6:00 p.m. - I stop and let it cool
7:00 p.m. - add 100ml of isopropanol, mix well (magnetic) and freeze.
09:00 a.m. - I start to filter by gravity the frozen product by mixing regularly
12:00 p.m. - transfer to a pyrex dish for the end of drying (in an incubator)
8:30 p.m. - weighed and transferred to the fridge, 67.7gr. - (71.11%)
55gr benzaldehyde
40gr nitroethane
10ml acid acetic 80°
3ml isopropanol 99.9%
10ml cyclohexylamine
2:20 p.m. - start of mixing, hotplate at maximum
2:28 p.m. - seems homogeneous to me, with small oily reflections but if I don't see any bubbles
2:32 p.m. - I see bubbles forming in the liquid
2:33 p.m. - I lower the temperature (as I usually do) and turn on the mixer, strong for a few minutes then reduce it a little
6:00 p.m. - I stop and let it cool
7:00 p.m. - add 100ml of isopropanol, mix well (magnetic) and freeze.
09:00 a.m. - I start to filter by gravity the frozen product by mixing regularly
12:00 p.m. - transfer to a pyrex dish for the end of drying (in an incubator)
8:30 p.m. - weighed and transferred to the fridge, 67.7gr. - (71.11%)
Second try with acid acetic :
55.4gr benzaldehyde
40.1gr nitroethane
11ml acid acetic 80°
5ml isopropanol 99.9%
10ml cyclohexylamine
same procedure, just waiting a little more little bubbles (a lot on my maggnetic stirrer) at the bigining
weighed and transferred to the fridge, 69.6gr. - (72.88%)
55.4gr benzaldehyde
40.1gr nitroethane
11ml acid acetic 80°
5ml isopropanol 99.9%
10ml cyclohexylamine
same procedure, just waiting a little more little bubbles (a lot on my maggnetic stirrer) at the bigining
weighed and transferred to the fridge, 69.6gr. - (72.88%)
at first I threw everything away... now I try to refreeze for the experiment; and this gives new crystals... sometimes even very long
but I don't know if it's a good product, I separate the refreezing from the rest of the harvest
The crystals look good. In the first crystallizations, there was little alcohol, so the sediment fell out densely.
