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

[ASheSChem]

hello,
i want to clearly understand this method before my first try :


with this method he don't speak about glacial acetic acid, it is normal ?

Ok, but.. we let it like that or we need to separate the 2 layers?

So.. it cristalized in the flask with all liquids (and no need freeze or something like that..?)
We don't need to filter the crystals before add the ethanol ?

that's it... Thank youuu

 

[HIGGS BOSSON]

It is better to add acetic acid, with it the condensation reaction of nitroethane and benzaldehyde will go better.

The results were 2 layers. One orange layer at the bottom with phenyl-2-nitropropene and a clear layer at the top with cyclohexylamine and maybe a little bit (~1mL) of H2O.

\\\\\\\\You can crystallize the whole RM, then wash the p2np crystals with cold alcohol (IPA), all the contaminants will go away. During condensation with acetic acid, the reaction mass is not divided into layers

So.. it crystallized in the flask with all liquids (and no need to freeze or something like that..?)
\\\\Usually, crystallization is easy when the mixture cools. But there are times when it is necessary to stimulate it. To do this, I use:
Freezing RM in the freezer
Addition of p2np crystals or NaCl
Transfusion from glass to glass of a small amount of solution to increase the site of contact with air

We don't need to filter the crystals before add the ethanol ?
\\\\\
You can do it in different ways. I would first filter out the crystals, then wash them with cold alcohol, and then recrystallize them from this alcohol.

 

[ASheSChem]

Thank a lot Higgs !
it's a little more clear in my head

 

[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 ?

 

[Mclssmxxl]

Flask on the right looks good to me, filter it and do recrystalization maybe?

 

[ASheSChem]

Hi guys, thanks for coming

So.... i have filter the yellow flask and junk the white one.

Spoiler: Pictures

it really takes a very long time to air dry. I'm waiting for it to be 100% dry to weigh.

any tips for a fast drying with no vaccum pump ?

edit : and do you think i need to recrystalize them?

 

[Mclssmxxl]

Don’t dry it yet, dissolve in hot (60-70 max) isopropanol, as little as possible.After all is dissolved let it sit at room temp preferably in dark for 24. Purity of substrate is pretty important, plus u get some nice looking crystals.Good job btw, looks like the real deal, just a bit crude.Also try to get your hands on a dean stark, theoretically I think yield is better the more water you remove.

 

[G.Patton]

How did you make filtration without vacuum pump? Via gravity filtration? You can use Water jet pump, it's extremely simple to use and quite cheap.

P.S. Good job

 

[Honolulu98]

Looks great! Sounds like you did a great job synthesizing. In a few weeks I want to synthesize a large amount of P2NP. Let's see if I get as good as you

 

[ASheSChem]

Thanks all for good vibes

ok thanks; need to dissolve it in isopropanol, and after 24, another filtering? freezing?

i don't know dean stark, i have never learn chemistry at school :'( i google that this night


yes by gravity, thanks for the water jet pump tips; need to learn that !


thanks a lot, hope you the best

 

[ASheSChem]

Sooooo i have trying to understand the dean stark but i have some questions..

if I understand correctly, with this assembly, the water vapor and cyclohexylamine will be separated from the rest?

do you think there are a lot of vapors at this temperature? (60-70°C)

so in the end, even without acetic acid, I will only get one layer?

no loss of product, only better quality?

 

[G.Patton]

yes
No, you can get crystalline impurities after freezing.

 

[ASheSChem]

Trying to continue;

So, i have put 50-60ml of isopropanol in my yellow powder, 60-70° and mixer

Spoiler: Pictures

now I'm waiting 24 hours...
I hope not to have lost too much product

 

[ASheSChem]

oops... I just realized that I filtered directly after heating and mixing...

I had to wait 24 hours?
big mistake?

 

[WillD]

No, save the filtered liquid and let crystallize too.

 

[ASheSChem]

Ok thanks, this is the actual result

Spoiler: Pictures

Sooo , i let dry all; keep all and it's my final p2np ?
or i need to purify another time?

sorry for a lot of noob questions , the second try will be more professional haha

 

[Mclssmxxl]

I think maybe you still have a lot of impurities because of how red your isopropanol got, I would do another, but it’s your call.It’s probably gonna yield something atleast if you wanna go at it.

 

[ASheSChem]

i need to let it dissolved 24h before filtering? right?

 

[Mclssmxxl]

Ideally yeah, but you can filter off some before 24h, reheat the leftover solution, evaporate a bit (fumes are irritant) and let that sit to recover the rest.

 

[ASheSChem]

Thanks for the support and help.
So I mixed all my product in 100ml of isopropanol at 60-70°C for 30-40 min. at rest I got 2 layers (no picture), a translucent orange and an opaque yellow.

now i'm waiting...
but after only one hour, I have the impression that the crystals are already forming.
I have the impression that it expands, inflates

Spoiler: Pictures

I have to leave the flask open for evaporation for 24 hours or not?
before filtering...