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Bhuro

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Reaction scheme:
View attachment 1298


Heat variant:
1. 1000 ml benzaldehyde, 1000 ml nitroethane, 250 ml glacial acetic acid and 50 ml n-butylamine was added in 10 L flask.
2. Install a 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 800 ml IPA in the bucket and stirred.
7. Put the bucket in the freezer for 12 hours.
8. After that time, P2NP was crystallized.
9. Filtered and dried.

Microwave variant:
1. 100 ml benzaldehyde, 100 ml nitroethane, 25 ml glacial acetic acid and 20 ml n-butylamine was added in 500 ml glass.
2. Put a rubber glove on a glass.
3. The glass was put in the microwave.
4. Turn on the power of 750 W 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 irradiations.
6. After that, add 100 ml IPA, stirred and put in the freezer for 12 hours.
7. After that time, P2NP was crystallized.
8. Filtered and dried.
William Dampier
 

BongMan

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how Much degree tem
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.
ASheSChem

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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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?)
MontecristoRead the thread. This has already been asked.
 

Sitr1x

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My friend, we can never get nitroethane, is there an alternative to it in this case?
cyb3r0Just 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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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.
Sitr1xWelcome
There is a thread on the forum for the synthesis of nitroethane
 

Mclssmxxl

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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.
Sitr1xSome 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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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.
MclssmxxlThat'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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Just wondering could this method be scaled down in half of the original amounts along with a 5litre flask used for example ?
Ta
Sitr1xBien 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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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
MclssmxxlThanks 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
 

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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
s3v3nYou can, but the results are worse, I never liked using acetate in this synthesis. Cyclohexylamine and butylamine are the best catalysts.
 

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

s3v3n

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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.
William Dampierwould 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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would it also be possible to use methylamin hcl as a catalyst, it would be much easier to get for me
s3v3nYes, 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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would it also be possible to use methylamin hcl as a catalyst, it would be much easier to get for me
s3v3nI'm not sure that methylamine base has enough base potency. You can try triethylamine or diethylamie.
 
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