1-Phenyl-2-nitropropene (P2NP) Video Synthesis From Benzaldehyde and Nitroethane. Henry Reaction.

[ASheSChem]

same dosage ?

 

[WillD]

Yes, use the same quantities.

 

[woohoo]

Look for pihkal and rhodium chemistry archive for more info on henry reaction catalyst.
Simple acetamide works too.

 

[ASheSChem]

can we use 80% acid acetic or only glacial ?

 

[WillD]

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.

 

[ASheSChem]

Ok, Thanks !

 

[ASheSChem]

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 ?

 

[WillD]

Mix everything and add isopropanol until the mixture becomes homogeneous. After add a little more for boils and start the reaction.

 

[ASheSChem]

Thank you very much I will also try this technique, we will see if I have a bigger harvest

 

[ASheSChem]

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%)

Spoiler: Photos

 

[flyhigh]

with same quantities can you suggest what quantity of n-butlyamine to be used ? instead of cyclohexylamine ?

 

[flyhigh]

is it 55grams benzaldehyde or 55ml ? coz density is 1.04gm/L and in the picture your flask size is 200ml , so im guessing it must be 55ml
please suggest

 

[ASheSChem]

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%)

 

[WillD]

Did you leave a filtrate in the freezer?

 

[ASheSChem]

what do you mean, re-freeze the liquid filtered another time?

 

[WillD]

yes

 

[ASheSChem]

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

 

[HIGGS BOSSON]

The crystals look good. In the first crystallizations, there was little alcohol, so the sediment fell out densely.

 

[yin-yang]

Can I use this for as a catalyst? N- is same as 1- right?

1-Butylamine
CAS no: 109-73-9

I know there are some isomers so wanna make sure this is the right one.

 

[yin-yang]

Also, I heard you can recover N-Butylamine and re-use it again. How to do that exacly?

 

[MadHatter]

You just distill it out. Boiling point 77-79 C.

 

[yin-yang]

quite close to isopropyl bp- 82.5. should i use fractional destination or regular can get job done ?