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1-Phenyl-2-nitropropene (P2NP) Video Synthesis From Benzaldehyde and Nitroethane. Henry Reaction.
- Thread starter GhostChemist
- Start date
Ive used the Nipron ®™ fuel enrichment additive cas 79-24-3 Pure nitroethane based, 100 ml with ammonium acetate and benzldehyde to produce p2np it seemed ok to me was just hard to crystalize. i just threw in a small cube of nitrogen to get it cold enough
I can't get cyclohexylamine nor butylamine but I can get ammonium acetate.
I'm going to do 100ml benzaldehyde, 100ml nitroethane and 25ml acetic acid.
So how much ammonium acetate will I need?
I'm going to do 100ml benzaldehyde, 100ml nitroethane and 25ml acetic acid.
So how much ammonium acetate will I need?
- By 41Dxflatline
Why can't you get them?
↑View previous replies…
- By 41Dxflatline
Ammonium Acetate Catalysis in Excess Nitroethane
A solution of benzaldehyde (6.4 g) and ammonium acetate (1.0 g) in nitroethane (20 mL) was heated to reflux for 5 h. On cooling, after removal of the solvent, the residue was purified by column chromatography on silica gel 60 N (neutral; hexane-chloroform, 2:1, v/v), then recrystallized from hexane and gave 1-phenyl-2-nitropropene as a light yellow crystals weighing 6.2g (63%), mp 71-73°C.
A solution of benzaldehyde (6.4 g) and ammonium acetate (1.0 g) in nitroethane (20 mL) was heated to reflux for 5 h. On cooling, after removal of the solvent, the residue was purified by column chromatography on silica gel 60 N (neutral; hexane-chloroform, 2:1, v/v), then recrystallized from hexane and gave 1-phenyl-2-nitropropene as a light yellow crystals weighing 6.2g (63%), mp 71-73°C.
- By yuiopjkl
Thank you. I have also read this method in previous replies.
And Someone in the replies said:
The thing that I understood is that if I add acetic acid, I will not need a high temperature, and the synthesis time will decrease.
If I did the same amount as in the thread said
100ml Benzaldehyde
100ml nitroethane
25ml Acetic acid
?? Ammonium acetate
how much ammonium acetate will I need?
Experts need your help please @G.Patton @HIGGS BOSSON
And Someone in the replies said:
The thing that I understood is that if I add acetic acid, I will not need a high temperature, and the synthesis time will decrease.
If I did the same amount as in the thread said
100ml Benzaldehyde
100ml nitroethane
25ml Acetic acid
?? Ammonium acetate
how much ammonium acetate will I need?
Experts need your help please @G.Patton @HIGGS BOSSON
I put 10ml benzaldehyde, 10ml nitroethane, 2.5ml GAA, and 4g ammonium acetate in a flask
Heating at 60-70 °C for 4 hours. After cooling to room temperature, there were two layers, at the bottom a yellow layer and at the top a white layer. I put it in an ice bath for 2 hours (I don't have access to a freezer right now) and there weren't any crystals, only the oily layer got thicker. The upper layer was discarded , 10 ml of distilled water was poured, and it was cooled in an ice bath for 5 hours. Nothing happened, only the aqueous layer became transparent.
The aqueous layer was discarded and 10 ml of IPA was poured. There are no layers, only one yellow layer.
It was placed in the freezer for 10 hours and there are no crystals .
Is there anything wrong with my method?
Sorry for my bad english
Heating at 60-70 °C for 4 hours. After cooling to room temperature, there were two layers, at the bottom a yellow layer and at the top a white layer. I put it in an ice bath for 2 hours (I don't have access to a freezer right now) and there weren't any crystals, only the oily layer got thicker. The upper layer was discarded , 10 ml of distilled water was poured, and it was cooled in an ice bath for 5 hours. Nothing happened, only the aqueous layer became transparent.
The aqueous layer was discarded and 10 ml of IPA was poured. There are no layers, only one yellow layer.
It was placed in the freezer for 10 hours and there are no crystals .
Is there anything wrong with my method?
Sorry for my bad english
Has it crystalized yet? The organic layer being at the bottom is good indication reaction has taken place esp. if you say it's yellow, if there was unreacted nitroethane it would float to the top of water.It might want more or less solvent.Another thing u can try is seeding with any crystal, NaCl for ex. after chill overnight. A small amount of finely crushed ice might also do it after a good chill.
For further reference primary amines can be obtained from commercially available amino acid supplements trough acid base extraction
For further reference primary amines can be obtained from commercially available amino acid supplements trough acid base extraction
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There was a little oil floating on top of the water
And there was a benzaldehyde smell
This picture after heating for four hours
Then separate the aqueous layer, pour IPA and Put it in the freezer for 10 hours
And this is after shaking
No crystals appeared, then I evaporated I PA at room temperature, added 2.5 ml of acetic acid, and put it in a water bath at 80°
I think I'll throw it away and try again
Should I put more acetic acid like 6ml
(10ml benzaldehyde,10ml nitroethane,6ml GAA, and 3g ammonium acetate)
- By yuiopjkl
There was a little oil floating on top of the water
And there was a benzaldehyde smell
This picture after heating for four hours
Then separate the aqueous layer, pour IPA and Put it in the freezer for 10 hours
And this is after shaking
No crystals appeared, then I evaporated I PA at room temperature, added 2.5 ml of acetic acid, and put it in a water bath at 80°
I think I'll throw it away and try again
Should I put more acetic acid like 6ml
(10ml benzaldehyde,10ml nitroethane,6ml GAA, and 3g ammonium acetate)
I think you should consider a traditional catalyst, like I said you can get it from aminoacid supplements.Also if there's an option I would go lower heat and more time rather than reverse.
After I have successfully carried out the synthesis as it was shown in the first video, I now have the final question:
What remains besides the product? How can I recycle it?
My mother liquor has two layers, a heavier dark red oily layer and an upper light yellow layer, I assume an IPA/water mixture, from which I could distill the IPA.
Is the lower dark red layer also still usable? Or just waste?
What remains besides the product? How can I recycle it?
My mother liquor has two layers, a heavier dark red oily layer and an upper light yellow layer, I assume an IPA/water mixture, from which I could distill the IPA.
Is the lower dark red layer also still usable? Or just waste?
Sounds like you have nitro left, mother liquid should be monophasic and if already red it is more than likely spent.You could add ipa to homogenize everything and toss in freezer
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- By ACAB
It was a mother liquor of two syntheses, the first of which gave nice pure yellow crystals and the second rather so slightly impure. As if the P2NP had been stored too long. I definitely need to do a recrystallization before I can use it. The second synthesis has been heating for more than 6 hours and was not directly processed further. So I am assuming oxidation rather than an Incomplete reaction..
My ratio
75ml Cyclohexamie
375ml Benzaldehyde
150ml Acetic acid
375ml Nitroethan
6h @ 60°C
1.Yield:550g
2. need recrystallization
But my question was more in the direction of how I can recover something from it.
I can distill IPA from the upper water.
From the red oil too, or does it go directly into the waste canister for incineration?
My ratio
75ml Cyclohexamie
375ml Benzaldehyde
150ml Acetic acid
375ml Nitroethan
6h @ 60°C
1.Yield:550g
2. need recrystallization
But my question was more in the direction of how I can recover something from it.
I can distill IPA from the upper water.
From the red oil too, or does it go directly into the waste canister for incineration?
about disposal? if you are in germany or austria you can take in chemical waste no questions asked for free.
Waste solvents can also be dilstilled for reuse, check the thread.
Waste solvents can also be dilstilled for reuse, check the thread.