Question P2NP synthesis

[Zeus the chemist]

I tried synthesizing P2NP using benzaldehyde and nitroethane, with cyclohexylamine catalyst. Refluxed it for 6 hours and got nothing. Just a yellow oil like substance that burns when set on fire. Can someone help me with this?

 

[wael gano]

What temperature did you use?
Did you add solvent?

 

[Zeus the chemist]

The instruction was to relfux at 60°C but our system couldn't handle it, so the temperature was about 80°C . And it reached 120°C as the time passed. We used a heating mantle, it doesn't have a setup to control temperature.

 

[wael gano]

It is necessary to add isopropyl alcohol to the reaction mass and heat it to 50 degrees Celsius, then put it in the freezer until crystals appear.

 

[Zeus the chemist]

Thank you for replying. Does the reaction work at 50°C? Should I reflux it for 6 hours at 50°C?

 

[wael gano]

You can use an oil or water bath at a constant temperature of 60/80
3 hours, then remove the heat and wait for it to cool. It is preferable to add IPA twice the weight of benzaldehyde
Place it in the freezer to crystallize

 

[Zeus the chemist]

I didn't use any solvent, it was a mixture of Benzaldehyde, cyclohexylamine and Nitroethane. In your opinion what solvent should I use?

 

[wael gano]

Add IPA solvent

 

[HIGGS BOSSON]

Show me a picture of your reaction mass.
Sometimes there are difficulties with crystallization. To start the process, it is necessary to cool in the freezer, and then add a grain of P2NP as an excitation of crystallization.
Sometimes it helps to pour the solution from a glass into a glass for oxidation.

 

[Zeus the chemist]

Thank you for replying. This is my first time synthesizing P2NP. I couldn't take a pic of. Also my temperature wasn't right, my system couldn't handle temperature of 60°C constant temperature. The temperature was 80°C and rose upto 120°C. It was constant at 120°C and never rose beyond that. Can you suggest a better way to synthesize it. I willing to try it till I get the right product.

 

[HIGGS BOSSON]

Look carefully our videos on the synthesis of P2NP

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/media/1-phenyl-2-nitropropene-synthesis.69/

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

Reaction scheme: Equipment and glassware: 10 L Flask; Retort stand and clamp for securing apparatus (optional); Reflux condenser; Funnel; Vacuum source; Laboratory scale (0.1-500 g is suitable) - optional; Measuring cylinders 1000 mL and 100 mL; Water bath; Glass rod and spatula; Filter...

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