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

[tankikan]

Reaction scheme:
View attachment 1298


Heat variant:
1. 1000ml benzaldehyde, 1000ml nitroethane, 250ml glacial acetic acid and 50ml n-butylamine was added in 10l flask.
2. Install condenser on the flask.
3. Start stirring and heat reaction mixture to 60*C.
4. Heating mixture 2-3 hours.
5. Empty mixture in the bucket.
6. Add 800ml IPA in the bucket and stirred.
7. Put the bucket in the freezer at 12 hours.
8. After that time P2NP was crystallized.
9. Filtered and dried.

Microwave variant:
1. 100ml benzaldehyde, 100ml nitroethane, 25ml glacial acetic acid and 20ml n-butylamine was added in 500ml glass.
2. Put a rubber glove on a glass.
3. The glass was put in the microwave.
4. Turn on the power of 750W and warm so much time so that the mixture does not boil.
5. We repeat the step 4 several times, let me cool the mixture. Minimum 6 irradiation.
6. After that, add 100ml IPA, stirred and put in the freezer for 12 hours.
7. After that time P2NP was crystallized.
8. Filtered and dried.

William DampierMay i know if Nitromethane is equal to nitroethane?

And is it possible to use this item (as attached screenshot) as n-butylamine? If yes, how would you suggest to proceed?

 

[MisterAnonymous]

May i know if Nitromethane is equal to nitroethane?

And is it possible to use this item (as attached screenshot) as n-butylamine? If yes, how would you suggest to proceed?

tankikanSend me a DM I will provide you with a contact for nitroethane and N-butylamine...

 

[rampage]

Hi
Not sure if this is the right section but does anyone know if this recipe will work?

Preparation of phenylnitropropanol:
Into a suitable beaker or conical flask place 51mls of benzaldehyde, followed by 33mls of nitroethane,
immediately thereafter add in 30 mls of a 30% potassium carbonate solution, rapidly stir the entire
mixture at room temperature for 2 hrs.
A cold water bath or ice bath may be needed to keep the reaction mixture at ambient temperature
(room temperature) or below. Do not allow the reaction mixture to get above 25 degrees celsius.
After stirring for 2 hrs add to the reaction mixture 200mls of diethyl ether, shortly thereafter add in
90mls of a 10% sodium bisulfite solution and moderately stir the entire reaction mixture for 30 minutes.
Afterwards place the entire reaction mixture into a seperatory funnel and remove the lower aqueous
layer, leave the ether layer in the seperatory funnel and wash the ether layer with 3 x 75ml portions of
cold water, each time removing the lower aqueous layer.
Place the ether layer into a suitable beaker or conical flask and add 15gms of anhydrous magnesium
sulfate and stir the entire mixture for 10 minutes to absorb any water in the ether. Then filter off the
magnesium sulfate.
Place the filtered ether mixture into a distallation apparatus and remove the ether, when no more ether
passes over or is collected allow the residue to cool to room temperature, then collect this residue as it
consists of the desired phenylnitropropanol.

 

[handle]

Hi
Not sure if this is the right section but does anyone know if this recipe will work?

Preparation of phenylnitropropanol:
Into a suitable beaker or conical flask place 51mls of benzaldehyde, followed by 33mls of nitroethane,
immediately thereafter add in 30 mls of a 30% potassium carbonate solution, rapidly stir the entire
mixture at room temperature for 2 hrs.
A cold water bath or ice bath may be needed to keep the reaction mixture at ambient temperature
(room temperature) or below. Do not allow the reaction mixture to get above 25 degrees celsius.
After stirring for 2 hrs add to the reaction mixture 200mls of diethyl ether, shortly thereafter add in
90mls of a 10% sodium bisulfite solution and moderately stir the entire reaction mixture for 30 minutes.
Afterwards place the entire reaction mixture into a seperatory funnel and remove the lower aqueous
layer, leave the ether layer in the seperatory funnel and wash the ether layer with 3 x 75ml portions of
cold water, each time removing the lower aqueous layer.
Place the ether layer into a suitable beaker or conical flask and add 15gms of anhydrous magnesium
sulfate and stir the entire mixture for 10 minutes to absorb any water in the ether. Then filter off the
magnesium sulfate.
Place the filtered ether mixture into a distallation apparatus and remove the ether, when no more ether
passes over or is collected allow the residue to cool to room temperature, then collect this residue as it
consists of the desired phenylnitropropanol.

rampageThe Nitroalkene can be reduced with Fe and HCl. >Here<

 

[BongMan]

The Nitroalkene can be reduced with Fe and HCl. >Here<
View attachment 38031

WhyTheFacereduction with Fe and Hcl creepy and not good for large scale use instead Tin(II)chloride it is easier and feasible on both lab and large scale.