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

[plancklong]

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]

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]

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...

 

[the money]

N-Butylamine

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

 

[UWe9o12jkied91d]

N-Butylamine

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

Foryoun-butil yes, di n-butil no

 

[the money]

This is available at Cyclohexylamine for synthesis, 500 ML

CAS No: 108-91-8

 

[UWe9o12jkied91d]

This is available at Cyclohexylamine for synthesis, 500 ML

CAS No: 108-91-8

ForyouYes

 

[the money]

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]

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]

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]

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]

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]

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

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

 

[G.Patton]

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]

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]

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]

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.