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

[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]

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

View attachment 4612 View attachment 4613 View attachment 4614 View attachment 4615

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

 

[flyhigh]

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

View attachment 4612 View attachment 4613 View attachment 4614 View attachment 4615

ASheSChemis 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

 

[ACAB]

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?

 

[UWe9o12jkied91d]

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?

ACABSounds 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

 

[ACAB]

you toss it and react fully next time, what is the ratios you used?

UWe9o12jkied91dAny advise? I would hate to dump everything into the environment and keep waste to a minimum.

 

[UWe9o12jkied91d]

Any advise? I would hate to dump everything into the environment and keep waste to a minimum.

ACABabout 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.

 

[Xiao hua]

Please tell me if it is cyclohexene or cyclohexamine? P2np synthesis video. Thanks

 

[UWe9o12jkied91d]

Please tell me if it is cyclohexene or cyclohexamine? P2np synthesis video. Thanks

Xiao huacyclohexene is not an amine

 

[Xiao hua]

cyclohexene is not an amine

UWe9o12jkied91dWhat is used in this video? Cyclohexene or cyclohaxamine

 

[Xiao hua]

What is used in this video? Cyclohexene or cyclohaxamine

Xiao huawhat chemical are instead of cyclohaxamine. cyclohaxamine is to get hard from my country. Asian

 

[UWe9o12jkied91d]

you may uses n-butlyamine if you are aisan

flyhighwhat if I'm black?

 

[flyhigh]

what if I'm black?

UWe9o12jkied91dammonium acetate output is so racemic

 

[oneimone]

Hi mates. i just need to make me sure that i can use any isomer of butylamine? I dont understand what means that small "n" before bunh2. Of course bunh2 and butanol is restricted in my country so i got to do it on my own. In UK once avaible to buy legal source of butanol is 2-butoxyethanol which i wanted brake with HCl and separate via distilation and later follow google patent to make bunh2, but im not sure i can use butan-2-ol. it is any difference between location OH group ?

 

[wael gano]

I tried the synthesis and I ended up with this solution. What is wrong with this? What do I do?

 

[UWe9o12jkied91d]

I tried the synthesis and I ended up with this solution. What is wrong with this? What do I do?

wael ganoyour solution seems to be inodorous, odorless and invisible

 

[wael gano]

 

[UWe9o12jkied91d]

View attachment 20176

wael ganoCan you describe procedure you did? Catalyst used, what stirring , what heating, reaction time etc.
Looks to me you got some product and the rest remained unreacted, but its just guess

 

[wael gano]

Can you describe procedure you did? Catalyst used, what stirring , what heating, reaction time etc.
Looks to me you got some product and the rest remained unreacted, but its just guess

UWe9o12jkied91dI tried the synthesis and I ended up with this solution. What is wrong with this? What do I do?
7.5 ml of benzaldehyde
6 ml of nitro ethane
3 ml of glacial acetic acid
1.8ml cyclohexylamine
Heating for 3,5 hours
What is wrong with the product of the reaction, something like the unreacted amine?

 

[wael gano]

لقد جربت التوليف وانتهى بي الأمر بهذا الحل. ما هو الخطأ في هذا؟ ماذا أفعل؟

 

[wael gano]

I tried the synthesis and I ended up with this solution. What is wrong with this? What do I do?
7.5 ml of benzaldehyde
6 ml of nitro ethane
3 ml of glacial acetic acid
1.8ml cyclohexylamine
Heating for 3,5 hours
What is wrong with the product of the reaction, something like the unreacted amine?

 

[UWe9o12jkied91d]

I tried the synthesis and I ended up with this solution. What is wrong with this? What do I do?
7.5 ml of benzaldehyde
6 ml of nitro ethane
3 ml of glacial acetic acid
1.8ml cyclohexylamine
Heating for 3,5 hours
What is wrong with the product of the reaction, something like the unreacted amine? View attachment 20179

wael ganohow much heat and with what? stirring?

 

[wael gano]

how much heat and with what? stirring?

UWe9o12jkied91dThe temperature is 60/80
I don't use a stirrer, I stir it from time to time

 

[UWe9o12jkied91d]

I tried the synthesis and I ended up with this solution. What is wrong with this? What do I do?
7.5 ml of benzaldehyde
6 ml of nitro ethane
3 ml of glacial acetic acid
1.8ml cyclohexylamine
Heating for 3,5 hours
What is wrong with the product of the reaction, something like the unreacted amine? View attachment 20179

wael ganooof, now I read carefully...you should use equal volumes of nitro benzo, that in your picture is unreacted benzaldehyde ofcourse

 

[flyhigh]

oof, now I read carefully...you should use equal volumes of nitro benzo, that in your picture is unreacted nitroethane ofcourse

UWe9o12jkied91dyoure right its a equimolar ratio of both but considering densities of benzaldehyde and nitroethane calculate the values of both appropriately

 

[777m]

possibly too long reaction time and amine degraded, plus it's about 3x the amine needed for that scale

UWe9o12jkied91dSo what do you think the real rates should be?

 

[UWe9o12jkied91d]

So what do you think the real rates should be?

777mproportions? equal volumes aldehyde alkene

 

[flyhigh]

how did you come up with those ratios ? those dont sound so stoichiometric to me.