# 1-Phenyl-2-nitropropene (P2NP) video synthesis from benzaldehyde and nitroethane. Henry reaction.



## GhostChemist

*Reaction scheme:*



​
*Equipment and glassware:*

10 L Flask;
Retort stand and clamp for securing apparatus (optional);
Reflux condenser;
Funnel;
Vacuum source;
Laboratory scale (0.1-500 g is suitable) - optional;
Measuring cylinders 1000 mL and 100 mL;
Water bath;
Glass rod and spatula;
Filter paper;
Laboratory grade thermometer; 
Buchner flask and funnel; 
Bucket 5-10 L.
Freezer;
*Reagents:*

Benzaldehyde 1000 ml; 
Nitroethane 1000 ml;
Glacial acetic acid 250 ml;
n-Butylamine 50 ml;
Isopropyl alcohol (IPA) ~1000 ml;










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1-Phenyl-2-nitropropene synthesis



__ Novator
__ Nov 20, 2022
__ 11
__
1-phenyl-2-nitropropene
amphetamine
benzaldehyde
cas 100-52-7
cas 705-60-2
henry reaction
nitroethane
p2np
p2np synthesis
phenyl-2-nitropropene video synthesis




Benzaldehyde and nitroethane Henry condensation...




*Medium scale:*
*1.* Benzaldehyde 1000 ml, nitroethane 1000 ml, glacial acetic acid 250 ml and n-butylamine 50 ml are placed into 10 L flask.
*2.* A reflux condenser is installed onto the flask.
*3.* The stirrer and heater are turned on. The reaction mixture is heated up to 60 °С.
*4.* The reaction is conducted during 2-3 hours with constant stirring at 60 °С.
*5.* The reaction mixture is poured into an empty 5-10 L bucket.
*6.* Isopropyl alcohol (IPA) 800 ml is poured into the bucket and stirred.
*7.* The bucket with mixture is put into a freezer for 12 hours, 1-phenyl-2-nitropropene (P2NP) is crystallized.
*8.* The product P2NP is filtered on a Buchner funnel (suction filtration procedure), washed be a small amount of cold IPA and dried on air (or in vacuum chamber, optional).​
*Equipment and glassware:*

Beaker 500 ml;
Funnel;
Vacuum source;
Laboratory scale (0.1-500 g is suitable) - optional;
Measuring cylinders 50 mL and 100 mL;
Glass rod and spatula;
Filter paper;
Buchner flask and funnel; 
Freezer;
Microwave oven 750 W;
*Reagents:*

Benzaldehyde 100 ml; 
Nitroethane 100 ml;
Glacial acetic acid 25 ml;
n-Butylamine 20 ml;
Isopropyl alcohol (IPA) ~150 ml;

*Microwave (small) scale:*
*1.* Benzaldehyde 100 ml, nitroethane 100 ml, glacial acetic acid 25 ml and n-butylamine 20 ml are placed into 500 ml beaker.
*2.* A rubber glove is put onto the beaker.
*3. *The beaker is put into a microwave oven.
*4.* The power of the microwave oven is set up on 750 W. Oven is turned on and the mixture is warmed until the boiling. The mixture is cooled down to the room temperature.
*5.* *Step 4 *is repeated several times. Minimum 6 times.
*6.* Next, IPA 100 ml is added, reaction mixture is stirred and put into a freezer for 12 hours. 1-Phenyl-2-nitropropene (P2NP) is crystallized.
*7. *The product P2NP is filtered on a Buchner funnel (suction filtration procedure), washed be a small amount of cold IPA and dried on air (or in vacuum chamber, optional).

1-Phenyl-2-nitropropene (P2NP) can be recrystallized from hexane, methanol, ethanol or isopropanol (IPA).​


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## tankikan

William Dampier said:


> *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?


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## William Dampier

tankikan said:


> May i know if Nitromethane is equal to nitroethane?



tankikanNo, these are different reagents. With nitromethane, we will get nitrostyrene. Nitromethane with some substituted benzaldehydes is suitable for the synthesis of the sources of a large class of substances, various psychedelic.


tankikan said:


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


No


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## Montecristo

What is the yield for the heat method?


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## William Dampier

thatfella said:


> What is the yield for the heat method?



thatfellabefore 1,5 kg


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## cyb3r0

My friend, we can never get nitroethane, is there an alternative to it in this case?


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## HIGGS BOSSON

cyb3r0 said:


> My friend, we can never get nitroethane, is there an alternative to it in this case?



cyb3r0Problems with nitroethane in Europe began back in 2007, then gradually all countries put restrictions on this valuable reagent. And now there are two ways: to look for suppliers in countries where there is weak legislation with a developed chemical industry, for example, Bangladesh, or to synthesize independently, the methodology for this we have proposed.


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## anotherNovice

I can find benzaldehyde for perfumery labeled CAS 100-57-2. Is this the same as required?


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## William Dampier

anotherNovice said:


> I can find benzaldehyde for perfumery labeled CAS 100-57-2. Is this the same as required?



anotherNovicebenzaldehyde *cas 100-52-7*


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## mactipo01

hello!!
whats is ipa?
and how much methanphetamine can i get with the process?
ty beforhand


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## mactipo01

where i can buy 10l flask?


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## HIGGS BOSSON

mactipo01 said:


> hello!!
> whats is ipa?
> and how much methanphetamine can i get with the process?
> ty beforhand



mactipo01In this topic, a method for obtaining phenylnitropropene, a precursor for the synthesis of amphetamine, is published. If you need methamphetamine, then look at the relevant topics. IPA - isopropyl alcohol






Methamphetamine synthesis from P2P by NaBH4 reduction. Medium-Scale.


Introduction. I represent to BB audience Methamphetamine synthesis method of 1-phenyl-2-propanon (P2P) reduction by NaBH4. Following method allows obtaining and large batches of product. The hardest problem of this method is the heat generating during exothermic reaction of imine reduction...




chemforum.info









Methamphetamine from ephedrine tablets


Extraction of pseudoephedrine from pharmaceutical (Sudafed) tablets. Pseudoephedrine was extracted from Sudafed tablets using ethanol, ethanol/methanol (90:10% vol/vol) and methylated spirits. The solvents were chosen with reference to the relevant clandestine literature. For each extraction...




chemforum.info









Methamphetamine synthesis from P2P via Aluminum amalgam


Reaction scheme: Equipment and glassware: 5 L Round bottom flask; Retort stand and clamp for securing apparatus (optional); Reflux condenser; Funnel; Sieve filter (kitchen grade is ok); Syringe or Pasteur pipette; pH indicator papers; Beakers (500 mL x2, 250 mL x2, 100 mL x2); Vacuum source...




chemforum.info


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## mactipo01

oh ty!!.. very nice....is very hard to learn this...and no simple to do it.
you perhaps
sell it? or know where i can buy some stimolant pills?


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## William Dampier

mactipo01 said:


> oh ty!!.. very nice....is very hard to learn this...and no simple to do it.
> you perhaps
> sell it? or know where i can buy some stimolant pills?



mactipo01Regarding this topic, we can help with the synthesis of P2NP. Other discussions in other topics


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## mactipo01

sorry, i'm new...what is simple method to synthesis meth? P2NP or from ephedrine tablets?


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## William Dampier

P2NP/Al/Hg, good route to start but difficult for large scales


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## a_king

how to get n-butylamen please


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## William Dampier

a_king said:


> how to get n-butylamen please



a_kingu can replace to cyclohexylamine


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## ASheSChem

hi guys; 
if we use cyclohexylamine, do we need glacial acetic acid ?


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## HIGGS BOSSON

ASheSChem said:


> hi guys;
> if we use cyclohexylamine, do we need glacial acetic acid ?



ASheSChemYes


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## ASheSChem

HIGGS BOSSON said:


> Yes



HIGGS BOSSONsame dosage ?


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## William Dampier

ASheSChem said:


> same dosage ?



ASheSChemYes, use the same quantities.


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## woohoo

a_king said:


> how to get n-butylamen please



a_kingLook for pihkal and rhodium chemistry archive for more info on henry reaction catalyst.
Simple acetamide works too.


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## ASheSChem

can we use 80% acid acetic or only glacial ?


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## William Dampier

ASheSChem said:


> can we use 80% acid acetic or only glacial ?



ASheSChemWhen using aqueous acetic acid, you will most likely have to use some alcohol all at once to dissolve the water, benzaldehyde, and nitroethane together.


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## ASheSChem

Ok, Thanks !


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## ASheSChem

William Dampier said:


> When using aqueous acetic acid, you will most likely have to use some alcohol all at once to dissolve the water, benzaldehyde, and nitroethane together



William Dampier
like 100 ml benzaldehyde, 100 ml nitroethane, 20 ml acetic acid 80%, 5ml isopropanol and 10ml (or 20ml?) cyclohexilamine in 1 L flask and reflux ?


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## William Dampier

ASheSChem said:


> like 100 ml benzaldehyde, 100 ml nitroethane, 20 ml acetic acid 80%, 5ml isopropanol and 10ml (or 20ml?) cyclohexilamine in 1 L flask and reflux ?



ASheSChemMix everything and add isopropanol until the mixture becomes homogeneous. After add a little more for boils and start the reaction.


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## ASheSChem

Thank you very much I will also try this technique, we will see if I have a bigger harvest


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## 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


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## ASheSChem

Second try with acid acetic :

55.4gr benzaldehyde
40.1gr nitroethane
11ml acid acetic 80°
5ml isopropanol 99.9%
10ml cyclohexylamine

same procedure, just waiting a little more little bubbles (a lot on my maggnetic stirrer) at the bigining

weighed and transferred to the fridge, 69.6gr. - (72.88%)


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## William Dampier

Did you leave a filtrate in the freezer?


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## ASheSChem

what do you mean, re-freeze the liquid filtered another time?


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## William Dampier

ASheSChem said:


> what do you mean, re-freeze the liquid filtered another time?



ASheSChemyes


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## ASheSChem

William Dampier said:


> Did you leave a filtrate in the freezer?



William Dampier
at first I threw everything away... now I try to refreeze for the experiment; and this gives new crystals... sometimes even very long

but I don't know if it's a good product, I separate the refreezing from the rest of the harvest


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## HIGGS BOSSON

ASheSChem said:


> at first I threw everything away... now I try to refreeze for the experiment; and this gives new crystals... sometimes even very long
> 
> but I don't know if it's a good product, I separate the refreezing from the rest of the harvest
> 
> View attachment 4664



ASheSChemThe crystals look good. In the first crystallizations, there was little alcohol, so the sediment fell out densely.


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## wannabeechemist

Can I use this for as a catalyst? N- is same as 1- right?

1-Butylamine
CAS no: 109-73-9

I know there are some isomers so wanna make sure this is the right one.


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## wannabeechemist

Also, I heard you can recover N-Butylamine and re-use it again. How to do that exacly?


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## MadHatter

wannabeechemist said:


> Also, I heard you can recover N-Butylamine and re-use it again. How to do that exacly?



wannabeechemistYou just distill it out. Boiling point 77-79 C.


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## wannabeechemist

quite close to isopropyl bp- 82.5. should i use fractional destination or regular can get job done ?


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## Bhuro

William Dampier said:


> *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


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## BongMan

how Much degree tem



ASheSChem said:


> 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..


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## ASheSChem

BongMan said:


> How much degree temperature you kept for reflex..



BongMan
like 60-70°C


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## quite

Thank you!


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## Montecristo

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?)


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## MadHatter

Montecristo said:


> 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.


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## Sitr1x

cyb3r0 said:


> 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.


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## Mclssmxxl

Sitr1x said:


> 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.


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## Sitr1x

Mclssmxxl said:


> 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


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## Sitr1x

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


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## Mclssmxxl

Sitr1x said:


> 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


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## Sitr1x

Mclssmxxl said:


> 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


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## s3v3n

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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## William Dampier

s3v3n said:


> 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.


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## 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?


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## plancklong

Hi s3v3n,



s3v3n said:


> 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.


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## William Dampier

plancklong said:


> 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.


s3v3n said:


> 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.


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## s3v3n

William Dampier said:


> 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


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## UWe9o12jkied91d

s3v3n said:


> 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.


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## G.Patton

s3v3n said:


> 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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## UWe9o12jkied91d

G.Patton said:


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



G.PattonAre you 100% sure secondary amines work? I've read they kinda do with bad yield.


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## G.Patton

UWe9o12jkied91d said:


> Are you 100% sure secondary amines work? I've read they kinda do with bad yield.



UWe9o12jkied91dNo, not 100%. I know that they work well as organic base agent to start electrophilic addition reactions. And much easier and cheaper to be bought.


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## s3v3n

if i cant use methylamin, can i synthesise butylamin or cyclohexylamin myself or is this very difficult? thanks


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## G.Patton

s3v3n said:


> if i cant use methylamin, can i synthesise butylamin or cyclohexylamin myself or is this very difficult? thanks



s3v3nYou can, but nobody do this. Much easy to buy.


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## s3v3n

G.Patton said:


> Much easy to buy.



G.Pattoncan you recommend any sources, i didnt find any right away


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## G.Patton

s3v3n said:


> can you recommend any sources, i didnt find any right away



s3v3nYou can open Listing and search around suppliers websites. I've seen something there.


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## wannabeechemist

That nitro group sucks up election density so much that you can even do this nitroaldol reaction reaction without any base catalyst. Methylamine can deprotonate nitroalkene. Ive tested works fine.


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## G.Patton

wannabeechemist said:


> That nitro group sucks up election density so much that you can even do this nitroaldol reaction reaction without any base catalyst. Methylamine can deprotonate nitroalkene. Ive tested works fine.



wannabeechemistWhat the yield did you get?


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## wannabeechemist

On par with butylamine 60% but I synthesized both nitroethane and benzaldhyde myself and didn't do a proper clean up.


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## MadHatter

elchapo said:


> We take a glass jar with a tight lid, the main thing is that it closes tightly. Or a flask with a rubber stopper. Then load the following reagents. 110 ml of benzaldehyde 100 ml of nitroethane 17 ml N-butylamine Mix well and close tightly to prevent air from entering. Then put the jar or flask in a dark (no direct sunlight. Usually a cupboard is enough) a warm place, preferably 30-35 degrees, but it will be enough, and 25 will just last longer. We leave for 7-9 days, daily slightly shaking in circular motions. After loading the reagents, the rm will turn cloudy yellow. The next day you will see the rm turn transparent yellow. On rm 4 it will still be brighter but also have a yellowish tinge and water droplets will float above or below day 7 rm will become diluted tea, which means everything can be frozen, but if the rm has not turned amber, let the tea continue to infuse. after, after filtering and drying, we put the jar in the sea for a day, recrystallization should be carried out. The yield was 138 g after recrystallization and drying



elchapo
You put the jar in the SEA?


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## Mo0odi

Can anyone provide me the CAS number for cyclohexylamine?


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## UWe9o12jkied91d

108-91-8 @Mo0odi 
--

I can confirm that secondary amines don't work so well.I did 250g scale with 10ml dibutylamine.Only slight yellowing after 3h @65-70.I decided to salvage the situation by adding monoethanoloamine at which point the RM darkened significantly and went turbid.I left it refluxing for an additional 20-30 minutes at high heat and turned it off letting it cool to room temp, pured over ipa, frozen.First milking got me around 170g of P2


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## Mo0odi

Thank you 
What do you mean by amines?


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## UWe9o12jkied91d

Mo0odi said:


> Thank you
> What do you mean by amines?



Mo0odiCompounds containing an NH group, derivatives of ammonia (NH3).A few examples : Methylamine. Hexamine, Amphetamine, dibutylamine.A primary amine is is a compound that has only one of the H's in NH3 replaced by something else ex. methylamine, while secondary amines have 2 of the H's replaced by something, for example Dibutylamine, this is explained simply, there is a bit more to it but just so you understand.

The message was meant for the thread anyways, not you.We were disscusing if secondary amines can catalyze this reaction from the topic, and I indeed confirmed dibutyialmine atleast dosen't work so well.


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## Mo0odi

@UWe9o12jkied91d 
Thanks for your explanation


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## KDR

Hi! What is your opinion about synthesis of benzaldehyde from styrene via ozonolysis? and Do you think is possible to sinth. bzdhd from salicylic acid or from phenol?


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## G.Patton

KDR said:


> Hi! What is your opinion about synthesis of benzaldehyde from styrene via ozonolysis? and Do you think is possible to sinth. bzdhd from salicylic acid or from phenol?



KDRHello, this topic about P2NP synthesis. You can make new theme with your question.


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## Fenster

Anyone tried Phenethylamine as the catalyst?


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## UWe9o12jkied91d

Fenster said:


> Anyone tried Phenethylamine as the catalyst?



FensterI'm betting yes provided it can be freebased, if you're getting it from supplements the binders may prevent this, keep us posted, I'm curious.I was halfway to using amphtamine base as a catalyst once when I was out of propene, this would also be interesting to know.


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## Evilcarrot2

Hi just a quick question:
I did 100ml nitroethane 
142ml benzaldehyde 
And after re crystallising p2np with IPA got 149.2g after 2 days in a vacuum dessicator at full vac and 2 days air dried. Does that sound about right yied or could it be improved 
Kind regards newb


----------



## Fenster

Evilcarrot2 said:


> Hi just a quick question:
> I did 100ml nitroethane
> 142ml benzaldehyde
> And after re crystallising p2np with IPA got 149.2g after 2 days in a vacuum dessicator at full vac and 2 days air dried. Does that sound about right yied or could it be improved
> Kind regards newb



Evilcarrot2You need to take the Molecular Mass of both Benzaldehyde and P2NP. 100g of Benzaldehyde is just under 1 mole, 100 grams of P2NP is around .7 of a mole. Meaning you got around 70% if theoretical yield.


----------



## Evilcarrot2

Fenster said:


> You need to take the Molecular Mass of both Benzaldehyde and P2NP. 100g of Benzaldehyde is just under 1 mole, 100 grams of P2NP is around .7 of a mole. Meaning you got around 70% if theoretical yield.



FensterThank you. I had 100ml of nitroethane and 1 mol=75g
So I increased benzaldehyde to be slight excess but I didn't know how to work out %yield. 
If that was the case I did 1.333333 mols of nitroethane


----------



## Evilcarrot2

I tried to work it out but struggled. 
So I used 1.3333333333 mols nitroethane 
And 1.338107802487749 mols of benzaldehyde being a very slight excess. Does that mean the nitroethane is my limiting factor. So is it yied/1.333333333?
Sorry once I get this down I won't ask the question again


----------



## Evilcarrot2

I think I get it. 
So it's 0.92 mol of p2np divide that by the 1.3333333 mols nitroethane and I get me %yield of 69.19%


----------



## Fenster

Yes. That's correct.


----------



## Charlie3

Hi is the cas number for the nitroethane 79-24-3?



William Dampier said:


> *Reaction scheme:*
> View attachment 1298​
> *Equipment and glassware:*
> 
> 10 L Flask;
> Retort stand and clamp for securing apparatus (optional);
> Reflux condenser;
> Funnel;
> Vacuum source;
> Laboratory scale (0.1-500 g is suitable) - optional;
> Measuring cylinders 1000 mL and 100 mL;
> Water bath;
> Glass rod and spatula;
> Filter paper;
> Laboratory grade thermometer;
> Buchner flask and funnel;
> Bucket 5-10 L.
> Freezer;
> *Reagents:*
> 
> Benzaldehyde 1000 ml;
> Nitroethane 1000 ml;
> Glacial acetic acid 250 ml;
> n-Butylamine 50 ml;
> Isopropyl alcohol (IPA) ~1000 ml;
> 
> *Medium scale:*
> *1.* Benzaldehyde 1000 ml, nitroethane 1000 ml, glacial acetic acid 250 ml and n-butylamine 50 ml are placed into 10 L flask.
> *2.* A reflux condenser is installed onto the flask.
> *3.* The stirrer and heater are turned on. The reaction mixture is heated up to 60 °С.
> *4.* The reaction is conducted during 2-3 hours with constant stirring at 60 °С.
> *5.* The reaction mixture is poured into an empty 5-10 L bucket.
> *6.* Isopropyl alcohol (IPA) 800 ml is poured into the bucket and stirred.
> *7.* The bucket with mixture is put into a freezer for 12 hours, 1-phenyl-2-nitropropene (P2NP) is crystallized.
> *8.* The product P2NP is filtered on a Buchner funnel (suction filtration procedure), washed be a small amount of cold IPA and dried on air (or in vacuum chamber, optional).​
> *Equipment and glassware:*
> 
> Beaker 500 ml;
> Funnel;
> Vacuum source;
> Laboratory scale (0.1-500 g is suitable) - optional;
> Measuring cylinders 50 mL and 100 mL;
> Glass rod and spatula;
> Filter paper;
> Buchner flask and funnel;
> Freezer;
> Microwave oven 750 W;
> *Reagents:*
> 
> Benzaldehyde 100 ml;
> Nitroethane 100 ml;
> Glacial acetic acid 25 ml;
> n-Butylamine 20 ml;
> Isopropyl alcohol (IPA) ~150 ml;
> 
> *Microwave (small) scale:*
> *1.* Benzaldehyde 100 ml, nitroethane 100 ml, glacial acetic acid 25 ml and n-butylamine 20 ml are placed into 500 ml beaker.
> *2.* A rubber glove is put onto the beaker.
> *3. *The beaker is put into a microwave oven.
> *4.* The power of the microwave oven is set up on 750 W. Oven is turned on and the mixture is warmed until the boiling. The mixture is cooled down to the room temperature.
> *5.* *Step 4 *is repeated several times. Minimum 6 times.
> *6.* Next, IPA 100 ml is added, reaction mixture is stirred and put into a freezer for 12 hours. 1-Phenyl-2-nitropropene (P2NP) is crystallized.
> *7. *The product P2NP is filtered on a Buchner funnel (suction filtration procedure), washed be a small amount of cold IPA and dried on air (or in vacuum chamber, optional).
> 
> 1-Phenyl-2-nitropropene (P2NP) can be recrystallized from hexane, methanol, ethanol or isopropanol (IPA).​



William Dampier


----------



## wannabeechemist

Yes, that's the right cas.


----------



## teodor

can hexamine (methenamine) be used for the synthesis


----------



## UWe9o12jkied91d

teodor said:


> can hexamine (methenamine) be used for the synthesis



teodorno, atleast not with acceptable yields. You could try to freebase amindoacid salts from supplements and such(just a theory). Or if you are in the EU I can ship some.


----------



## Fenster

I've even heard some have had such with GABA.


----------



## G.Patton

Cheers! New video is here!


----------



## Mr.Blanks00

Evilcarrot2 said:


> Thank you. I had 100ml of nitroethane and 1 mol=75g
> So I increased benzaldehyde to be slight excess but I didn't know how to work out %yield.
> If that was the case I did 1.333333 mols of nitroethane



Evilcarrot2hello bad potato, are you using a cyclohexamine catalyst, or n butylamine.


----------



## Evilcarrot2

Hi I'm using butylamine.


----------



## Mr.Blanks00

Evilcarrot2 said:


> Hi I'm using butylamine.



Evilcarrot2Oh ok friends,thanks .


----------



## MadHatter

Honestly, is there any advantage to any of the catalysts? Is n-butylamine better than cyclohexylamine or is it vice versa? Or better and better- do they modify the reaction in terms of yield, sensitivity or robustness in any way? Which one would our experts choose if they had both?


----------



## UWe9o12jkied91d

MadHatter said:


> Honestly, is there any advantage to any of the catalysts? Is n-butylamine better than cyclohexylamine or is it vice versa? Or better and better- do they modify the reaction in terms of yield, sensitivity or robustness in any way? Which one would our experts choose if they had both?



MadHatterI'm no expert by any means but I've tried : n-butyl, cyclohexil, monoetanolo, NaOH, Dibutil. All primary amines worked great, everything else was not acceptable, so chose the least stinky primary amine I guess.


----------



## Felix34-73

Can methanol or ethanol be used instead of n-butylamine?
@G.Patton 
Fenster​


----------



## Marvin "Popcorn" Sutton

Felix34-73 said:


> Can methanol or ethanol be used instead of n-butylamine?



Felix34-73n-butylamine is a catalyst, it can be replaced by cyclohexylamine


----------



## cjcb[eqhfkbyf

Hello everyone!Too huge proportions Please tell me for 200 ml of benzaldehyde and nitroethane how much vinegar and isoproponal you need acetamide, if it is possible, how much to use?


----------



## HairyPoppins

plancklong said:


> 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.



plancklongIve 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


----------



## plancklong

cyb3r0 said:


> My friend, we can never get nitroethane, is there an alternative to it in this case?



cyb3r0I have been able to get this from ebay: 




Click here


----------



## HairyPoppins

plancklong said:


> I have been able to get this from ebay: View attachment 8222
> 
> Click here



plancklongive ordered that and the tip blender he sells, it comy from a chemical manufacture called eurchem spelled exactly like that.it is high quality,


----------



## HairyPoppins

plancklong said:


> I have been able to get this from ebay: View attachment 8222
> 
> Click here



plancklongThe problem is this part! this means your address could be compromised! Be careful


transport packaging certification
standardization
note:
:
:
:
:
:

​according to government transport ( IATA, ADR , ECHA-REACH ) rules
special for chemical transport
C.O.A., MSDS, GMP, API, USP, EUP, ECHA-REACH, ORIGIN, etc... *
*(originals will be delivered with good, and copies after confirmed order)
according to E.U. - Echa-Reach rules
the price of the product is already discounted less than -25% compared to the official price in force of the “ International Stock Exchange of chemical and pharmaceutical products ”, issued by ICIS


----------



## Pavel

As a curiosity, it also succeeded at room temperature. but that's a few dozen days. With the use of cyclohexylamine, But do not remember use glacial acetic acid...


----------



## Foryou

N-Butylamine

I got this
Di n butylamine
CAS:111-92-2
Can i use it


----------



## UWe9o12jkied91d

Foryou said:


> N-Butylamine
> 
> I got this
> Di n butylamine
> CAS:111-92-2
> Can i use it



Foryoun-butil yes, di n-butil no


----------



## Foryou

This is available at Cyclohexylamine for synthesis, 500 ML

CAS No: 108-91-8


----------



## UWe9o12jkied91d

Foryou said:


> This is available at Cyclohexylamine for synthesis, 500 ML
> 
> CAS No: 108-91-8



ForyouYes


----------



## Foryou

Are these reagents true or false? I want your help in obtaining a CAS number


----------



## MadHatter

Gaaaah. I managed to screw up the reaction this time and left the rm unattended for two hour. When I got back it was well over 110 C, probably had been for some time, and dark reddish-brown, with a very distinct smell that's difficult to describe. What do you think, did I burn this batch? If I manage to get anything to crystallize out of it, is it even trustworthy? 

I HAVE to get me a heating plate with better temp control.


----------



## UWe9o12jkied91d

MadHatter said:


> Gaaaah. I managed to screw up the reaction this time and left the rm unattended for two hour. When I got back it was well over 110 C, probably had been for some time, and dark reddish-brown, with a very distinct smell that's difficult to describe. What do you think, did I burn this batch? If I manage to get anything to crystallize out of it, is it even trustworthy?
> 
> I HAVE to get me a heating plate with better temp control.



MadHatterIs the smell like benzaldehyde but more nutty?
Anyways, wouldnt hurt to try crystalize it, see what comes out lol


----------



## MadHatter

Nah, no benzaldehyde smell anymore. Left it standing outside (under plastic film) in cold winter temp, no crystals. This is probably crap. Dammit.


----------



## MadHatter

Actually, scratch that! It's crystallized fine overnight. But there's this brown slurry around the yellow crystals and it definately smells bad. 
I made another batch without any temperature fuckups (actually ,using a sous-vide heater stick is a perfect heating system for this synth! Keeps a perfect, circulated water bath at an exact temperature, just a tip.). Now the second batch consists almost solely of solid, perfect yellow crytals. 

But for the bad batch: I want to clean it up properly. But finding solubility- or rather INSOLUBILTY data for P2NP is hard. Remind me @G.Patton @William Dampier etc, is P2NP insoluble in water? Apparently its perfectly soluble in both methanol and DCM.- how about non-polars? Like toluene? Could I wash it with that? What would the best clean-up procedure be? 
Recrystallizing from IPA apart, I mean.


----------



## UWe9o12jkied91d

MadHatter said:


> Actually, scratch that! It's crystallized fine overnight. But there's this brown slurry around the yellow crystals and it definately smells bad.
> I made another batch without any temperature fuckups (actually ,using a sous-vide heater stick is a perfect heating system for this synth! Keeps a perfect, circulated water bath at an exact temperature, just a tip.). Now the second batch consists almost solely of solid, perfect yellow crytals.
> 
> But for the bad batch: I want to clean it up properly. But finding solubility- or rather INSOLUBILTY data for P2NP is hard. Remind me @G.Patton @William Dampier etc, is P2NP insoluble in water? Apparently its perfectly soluble in both methanol and DCM.- how about non-polars? Like toluene? Could I wash it with that? What would the best clean-up procedure be?
> Recrystallizing from IPA apart, I mean.



MadHatterinsoluble in water, readily soluble in non-polar


----------



## MadHatter

UWe9o12jkied91d said:


> insoluble in water, readily soluble in non-polar



UWe9o12jkied91dActually, do you have a source? Because I can't find any real solubility data online, which vexes me.
And it's appparently soluble in ethanol and other spirits, so that sounds like it could be water soluble also?


----------



## UWe9o12jkied91d

MadHatter said:


> Actually, do you have a source? Because I can't find any real solubility data online, which vexes me.
> And it's appparently soluble in ethanol and other spirits, so that sounds like it could be water soluble also?



MadHatterYes, my source is it came to me in a dream


----------



## MadHatter

UWe9o12jkied91d said:


> Yes, my source is it came to me in a dream



UWe9o12jkied91dHa. Ha. Ok. Well, luckily there are other sources of information.


----------



## G.Patton

MadHatter said:


> Actually, scratch that! It's crystallized fine overnight. But there's this brown slurry around the yellow crystals and it definately smells bad.
> I made another batch without any temperature fuckups (actually ,using a sous-vide heater stick is a perfect heating system for this synth! Keeps a perfect, circulated water bath at an exact temperature, just a tip.). Now the second batch consists almost solely of solid, perfect yellow crytals.
> 
> But for the bad batch: I want to clean it up properly. But finding solubility- or rather INSOLUBILTY data for P2NP is hard. Remind me @G.Patton @William Dampier etc, is P2NP insoluble in water? Apparently its perfectly soluble in both methanol and DCM.- how about non-polars? Like toluene? Could I wash it with that? What would the best clean-up procedure be?
> Recrystallizing from IPA apart, I mean.



MadHatter





Phenyl-2-nitropropene


General information 1-Phenyl-2-nitropropene, or simply phenyl-2-nitropropene, or P2NP, as it is commonly referred to, is a chemical compound from the aromatic group of compounds, with the formula C9H9NO2. It is a light-yellow crystalline solid with a distinct smell. Phenyl-2-nitropropene is used...




bbgate.com


----------



## MadHatter

So here's the picture. Canary yellow crystals from perfect temperature control to the left, darker yellow ones to the right, from the run which went well over 110 C for quite some time.

Best cleanup now? Recrystallize from methanol or IPA?


----------



## UWe9o12jkied91d

MadHatter said:


> So here's the picture. Canary yellow crystals from perfect temperature control to the left, darker yellow ones to the right, from the run which went well over 110 C for quite some time.
> 
> Best cleanup now? Recrystallize from methanol or IPA?



MadHatterYes, maybe you can get away with a wash with minimal cold ipa or acetone.But a recrystalization in solvents you mentioned or, even better, ethyl acetate is ideal


----------



## G.Patton

MadHatter said:


> So here's the picture. Canary yellow crystals from perfect temperature control to the left, darker yellow ones to the right, from the run which went well over 110 C for quite some time.
> 
> Best cleanup now? Recrystallize from methanol or IPA?



MadHatterProduct can be recrystallized from hexane, methanol, ethanol, isopropanol


----------



## MadHatter

G.Patton said:


> Product can be recrystallized from hexane, methanol, ethanol, isopropanol



G.Patton So I opted for recrystallization from methanol Colour difference is still s´there, but slightly less so. Itäs a bitch getting the methanol out of the crystals though, I've been tampering with vacuum drying all day. 

But I have moved on to the reduction phase with NaBH4, now have a bottle of formylamphetamine in acetone over MgSO4 standing in the fridge for salting tomorrow. I jut need to get a clean, good salting acid, which I sadly don't have right now.


----------



## MadHatter

Actually, scratch that! It's crystallized fine overnight. But there's this brown slurry around the yellow crystals and it definately smells bad. 
I made another batch without any temperature fuckups (actually ,using a sous-vide heater stick is a perfect heating system for this synth! Keeps a perfect, circulated water bath at an exact temperature, just a tip.). Now the second batch consists almost solely of solid, perfect yellow crytals. 

But for the bad batch: I want to clean it up properly. But finding solubility- or rather INSOLUBILTY data for P2NP is hard. Remind me @G.Patton @William Dampier etc, is P2NP insoluble in water? Apparently its perfectly soluble in both methanol and DCM.- how about non-polars? Like toluene? Could I wash it with that? What would the best clean-up procedure be? 
Recrystallizing from IPA apart, I mean.


----------



## G.Patton

MadHatter said:


> Actually, scratch that! It's crystallized fine overnight. But there's this brown slurry around the yellow crystals and it definately smells bad.
> I made another batch without any temperature fuckups (actually ,using a sous-vide heater stick is a perfect heating system for this synth! Keeps a perfect, circulated water bath at an exact temperature, just a tip.). Now the second batch consists almost solely of solid, perfect yellow crytals.
> 
> But for the bad batch: I want to clean it up properly. But finding solubility- or rather INSOLUBILTY data for P2NP is hard. Remind me @G.Patton @William Dampier etc, is P2NP insoluble in water? Apparently its perfectly soluble in both methanol and DCM.- how about non-polars? Like toluene? Could I wash it with that? What would the best clean-up procedure be?
> Recrystallizing from IPA apart, I mean.



MadHatter





Phenyl-2-nitropropene


General information 1-Phenyl-2-nitropropene, or simply phenyl-2-nitropropene, or P2NP, as it is commonly referred to, is a chemical compound from the aromatic group of compounds, with the formula C9H9NO2. It is a light-yellow crystalline solid with a distinct smell. Phenyl-2-nitropropene is used...




bbgate.com


----------



## MadHatter

So here's the picture. Canary yellow crystals from perfect temperature control to the left, darker yellow ones to the right, from the run which went well over 110 C for quite some time.

Best cleanup now? Recrystallize from methanol or IPA?


----------



## G.Patton

MadHatter said:


> So here's the picture. Canary yellow crystals from perfect temperature control to the left, darker yellow ones to the right, from the run which went well over 110 C for quite some time.
> 
> Best cleanup now? Recrystallize from methanol or IPA?



MadHatterProduct can be recrystallized from hexane, methanol, ethanol, isopropanol


----------



## MadHatter

G.Patton said:


> Product can be recrystallized from hexane, methanol, ethanol, isopropanol



G.Patton So I opted for recrystallization from methanol Colour difference is still s´there, but slightly less so. Itäs a bitch getting the methanol out of the crystals though, I've been tampering with vacuum drying all day. 

But I have moved on to the reduction phase with NaBH4, now have a bottle of formylamphetamine in acetone over MgSO4 standing in the fridge for salting tomorrow. I jut need to get a clean, good salting acid, which I sadly don't have right now.


----------



## Dreadnsalty

GhostChemist said:


> *Reaction scheme:*
> View attachment 1298​
> *Equipment and glassware:*
> 
> 10 L Flask;
> Retort stand and clamp for securing apparatus (optional);
> Reflux condenser;
> Funnel;
> Vacuum source;
> Laboratory scale (0.1-500 g is suitable) - optional;
> Measuring cylinders 1000 mL and 100 mL;
> Water bath;
> Glass rod and spatula;
> Filter paper;
> Laboratory grade thermometer;
> Buchner flask and funnel;
> Bucket 5-10 L.
> Freezer;
> *Reagents:*
> 
> Benzaldehyde 1000 ml;
> Nitroethane 1000 ml;
> Glacial acetic acid 250 ml;
> n-Butylamine 50 ml;
> Isopropyl alcohol (IPA) ~1000 ml;
> 
> 
> 
> 
> 
> 
> 
> 
> 
> 
> Your browser is not able to display this video.
> 
> 
> Download Video
> 
> 
> 
> 
> 
> 
> 1-Phenyl-2-nitropropene synthesis
> 
> 
> 
> __ Novator
> __ Nov 20, 2022
> __ 11
> __
> 1-phenyl-2-nitropropene
> amphetamine
> benzaldehyde
> cas 100-52-7
> cas 705-60-2
> henry reaction
> nitroethane
> p2np
> p2np synthesis
> phenyl-2-nitropropene video synthesis
> 
> 
> 
> 
> Benzaldehyde and nitroethane Henry condensation...
> 
> 
> 
> 
> *Medium scale:*
> *1.* Benzaldehyde 1000 ml, nitroethane 1000 ml, glacial acetic acid 250 ml and n-butylamine 50 ml are placed into 10 L flask.
> *2.* A reflux condenser is installed onto the flask.
> *3.* The stirrer and heater are turned on. The reaction mixture is heated up to 60 °С.
> *4.* The reaction is conducted during 2-3 hours with constant stirring at 60 °С.
> *5.* The reaction mixture is poured into an empty 5-10 L bucket.
> *6.* Isopropyl alcohol (IPA) 800 ml is poured into the bucket and stirred.
> *7.* The bucket with mixture is put into a freezer for 12 hours, 1-phenyl-2-nitropropene (P2NP) is crystallized.
> *8.* The product P2NP is filtered on a Buchner funnel (suction filtration procedure), washed be a small amount of cold IPA and dried on air (or in vacuum chamber, optional).​
> *Equipment and glassware:*
> 
> Beaker 500 ml;
> Funnel;
> Vacuum source;
> Laboratory scale (0.1-500 g is suitable) - optional;
> Measuring cylinders 50 mL and 100 mL;
> Glass rod and spatula;
> Filter paper;
> Buchner flask and funnel;
> Freezer;
> Microwave oven 750 W;
> *Reagents:*
> 
> Benzaldehyde 100 ml;
> Nitroethane 100 ml;
> Glacial acetic acid 25 ml;
> n-Butylamine 20 ml;
> Isopropyl alcohol (IPA) ~150 ml;
> 
> *Microwave (small) scale:*
> *1.* Benzaldehyde 100 ml, nitroethane 100 ml, glacial acetic acid 25 ml and n-butylamine 20 ml are placed into 500 ml beaker.
> *2.* A rubber glove is put onto the beaker.
> *3. *The beaker is put into a microwave oven.
> *4.* The power of the microwave oven is set up on 750 W. Oven is turned on and the mixture is warmed until the boiling. The mixture is cooled down to the room temperature.
> *5.* *Step 4 *is repeated several times. Minimum 6 times.
> *6.* Next, IPA 100 ml is added, reaction mixture is stirred and put into a freezer for 12 hours. 1-Phenyl-2-nitropropene (P2NP) is crystallized.
> *7. *The product P2NP is filtered on a Buchner funnel (suction filtration procedure), washed be a small amount of cold IPA and dried on air (or in vacuum chamber, optional).
> 
> 1-Phenyl-2-nitropropene (P2NP) can be recrystallized from hexane, methanol, ethanol or isopropanol (IPA).​



GhostChemistI am getting 2 separate layers during reflux. One darker amber on top and a smaller layer that is a light yellow on bottom. This along with a white precipitate on bottom as well. Is this normal?


----------



## UWe9o12jkied91d

Dreadnsalty said:


> I am getting 2 separate layers during reflux. One darker amber on top and a smaller layer that is a light yellow on bottom. This along with a white precipitate on bottom as well. Is this normal?



DreadnsaltyLayers mean water, is your GAA pure? 
the white precipitate might be your product, does it dissolve on heating?


----------



## Dreadnsalty

UWe9o12jkied91d said:


> Layers mean water, is your GAA pure?
> the white precipitate might be your product, does it dissolve on heating?



UWe9o12jkied91dBrand new bottle of GAA at 99.85% purity. RM does smell strongly of GAA though. I will check product dissolve as soon as it gets done crystalizing out (hopefully)


----------



## BrownRiceSyrup

This reaction generates water right? Is there a way to remove the water to drive the reaction? I remember i saw somewhere someone used toluene as a solvent and used a dean start to remove the water but heat goes up to the 86 or whatever the azeotrope is with toluene. Is there anything wrong with that idea? Would that increase yield maybe?


----------



## G.Patton

BrownRiceSyrup said:


> This reaction generates water right? Is there a way to remove the water to drive the reaction? I remember i saw somewhere someone used toluene as a solvent and used a dean start to remove the water but heat goes up to the 86 or whatever the azeotrope is with toluene. Is there anything wrong with that idea? Would that increase yield maybe?



BrownRiceSyrup


> This reaction generates water right?


Hello, yes.


----------



## Hank Schrader

When we produced phenylnitropropene, we did not use heating.
Poured into a flask
nitroethane+benzaldehyde+catalyst was closed and left at room temperature.
The flask was shaken once a day. After 8 days, the solution was poured into water ... and propene crystals fell immediately to the bottom. The water was decanted and crystallized in alcohol.

If someone wants to get very high quality propene,
I will give you the technology below:

1 mole benzaldehyde
1,2 mole of nitroethane
+ 18ml n-butylamine

Put this in a glass bottle and close it.
Shake hard a couple of times a day.
After 8 days, open the bottle and pour 1 liter into a container of hot water.
Shake... drain the water, repeat the procedure with 500 ml of water.
Pour phenylnitropropene with alcohol and heat until completely dissolved and leave in the freezer.
Propene is obtained by this method practically without color.
The color is transparent yellow, the structure is like crystal methamphetamine.

According to my method, it will turn out ~ 135-140g


----------

