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

Bhuro

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BongMan

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how Much degree tem


How much degree temperature you kept for reflex..
 

quite

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Thank you!
 

Montecristo

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i can only get 50% acetic acid locally, can i use this? if so, what changes would i make ( heat method ).
I know acetic acid can be a pain to get fully concentrated, is there a way to push it up to 80%?
Or can another acid be used?
Also are there any risks i should know about? (explosive/toxic fumes?)
 

MadHatter

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Read the thread. This has already been asked.
 

Sitr1x

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Just a heads up SWIM found out on the clearweb somewhere that particular 'paint brush saver' liquids contain primarily Nitroethane and isn't too much on the expensive side of things.
 

wael gano

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Welcome
There is a thread on the forum for the synthesis of nitroethane
 

Mclssmxxl

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Some people report it’s not etno2, I don’t remember why or where I read it but I bet I can dig it up.
Either way great scheme to divert nitroethane if they’re replacing it with something else.
 

Sitr1x

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That's a shame =(

Might have to order some soon to do a test run using this method to see if it is legit ETNO2. I did read one post of someone claiming they have used it with no issue to produce P2NP so who knows. Wish I had an easy way of making it myself
 

Sitr1x

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Just wondering could this method be scaled down in half of the original amounts along with a 5litre flask used for example ?
Ta
 

Mclssmxxl

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Bien sûr.100g of your alkene can be reacted scaling reagent linearlly, except maybe less ipa idk exactly I go by eye, in a 1L erlenmeyer no problem.I reckon your could push 200 but overfilling past a certain point is not kosher
 

Sitr1x

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Thanks will scale down linearly and give it a try
 

s3v3n

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I read somewhere that ammonium acetat can be used as a catalyst in Henry reactions, can i use it here in the microwave method an what amount would i need? Thanks
 

WillD

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You can, but the results are worse, I never liked using acetate in this synthesis. Cyclohexylamine and butylamine are the best catalysts.
 

Kvadprime

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From the bases I have aniline, do you have information on the yields for aniline as the base catalyst?
 

s3v3n

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i found a method where you leave the benzaldehyde and nitroethan solution with methylamin as catalyst in a dark place for 2 weeks and they reported higher yields, has anyone here tryed that before or knows if this could work?
 

plancklong

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Hi s3v3n,
I did try this using benzaldehyde, nitroethane, and n-butylamine. As a template, I used 3,4-DMA from PIHKAL. Instead of the veratraldehyde and n-amylamine, I used benzaldehyde and n-butylamine, and adjusted the amounts accordingly.

The RM seems unchanged after a month. No solids have precipitated at all.

This was my last effort in a line of unsuccessful reactions with this nitroethane:

Nipron ®™ fuel enrichment additive cas 79-24-3 Pure nitroethane based, 100 ml.

This was supposed to be >98% nitroethane (NE). I didn't have any way to definitively check it, so it could be something other than NE or have high water content. Was expensive too - $125 for 100mL delivered.

I think this reaction (and I thought it was a Knovenagle reaction, not a Henry reaction!) would work, but there may be something about the unsubstituted benzaldehyde that requires different reaction conditions.
 

WillD

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Use the proportions and conditions written in this topic, it works optimally.
Made by various routes. Butylamine and cyclohexylamine are the best catalysts for this process.
 

s3v3n

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would it also be possible to use methylamin hcl as a catalyst, it would be much easier to get for me
 

UWe9o12jkied91d

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Yes, ethylamine also works ok.

EDIT: Oh you said HCl, that will not work, you need to add alkali solution to it to obtain the freebase methylamine then use as in procedure.
 

G.Patton

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I'm not sure that methylamine base has enough base potency. You can try triethylamine or diethylamie.
 
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