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

[plancklong]

I have been able to get this from ebay:

Click here

 

[HairyPoppins]

ive 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]

The 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-butil yes, di n-butil no

 

[the money]

This is available at Cyclohexylamine for synthesis, 500 ML

CAS No: 108-91-8

 

[UWe9o12jkied91d]

Yes

 

[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]

Is 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]

insoluble in water, readily soluble in non-polar

 

[MadHatter]

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?

 

[UWe9o12jkied91d]

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

 

[MadHatter]

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

 

[G.Patton]

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]

Yes, 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]

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

 

[MadHatter]

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.