Need help for a P2NP method + First try (pics)

[ASheSChem]

Hi guys...
So... I have try with what i have in stock.

Fiiiiiirst try, totally noob

To 55 g (0.5mol) Benzaldehyde in a 500mL Flask were added 40 g (0.5mol) Nitroethane and 10mL Cyclohexylamine. All was refluxed for 6h on a water bath. The result were 2 layers.

Spoiler: Pictures

after that, cooling at room temperature...

Spoiler: Pictures

after, 50mL of H2O were added and then sucked off with a pipette, 4 times.... but nothing happens, except reforming of 2 layers... (no photo sorry)

after, i have separate the 2 layers, and put 50ml of isopropanol in the orange one

Spoiler: Pictures

and i put it in the freezer... (actually 11h)

Spoiler: Pictures

to be continued...

 

[damian.dass]

Hi,can i know what's the temperature to freeze ?

 

[Evilcarrot2]

Just wanna add an update on a similar synthesis.
I mixed,
142 benzaldehyde
100ml nitroethane
7ml n-butylamine

And mixed at room temperature for 6 hours.
Observed a nice orange color so added 100ml of IPA and put in the freezer over night.
I awoke to an ice cold mixture of 0 crystals.

So not 1 to give up I removed RM from freezer and place in a rb flask on a water bath and added a reflux condenser.
When it started refluxing not sure on exact temp but about 80 degrees celcius I added 25ml of Gaa and continued for 4 hours.

After reflux I placed straight into freezer to awake to a solid mass of dirty crystals

Filtered them on a buchner with vacuum and wased with cold IPA.

put 100ml of IPA in a beaker and added all washed crystals and heated until all had dissolved at about 70-80 degrees celcius and placed back in freezer.

Within minutes I'm getting needle like crystals forming will post total weight after fully getting down to temperature and re filtering and drying.

Just wanted to add this to tell people not to give up on RM if you don't get crystals 1st time. I will add a pick of crystals formed so far!

 

[Evilcarrot2]

 

[Evilcarrot2]

Before put into desicator

 

[TotalSynthesis]

Hi,

with n-butylamine at room temperature is actually my preferred method because it's yields are perfect and your product will be that clean that recrystallization wont be needed at all.

The reason it did not work for you, is because of time. without external heating you just have to let it sit at a dark place for about 5-6 days and then everything will already be crystallized without cooling.

 

[Evilcarrot2]

Thanks for your reply unfortunately being my first actual p2np I was impatient but duely noted. Will try different routes when I locate more nitro ethane

 

[TotalSynthesis]

well, i can understand that. often times I also do not want to wait that long. but if time does not matter, i always prefer n-butylamine at rt