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

[HIGGS BOSSON]

Now you got pure crystals, and all the impurities remained in the alcohol solution. After crystallization, you can filter.

 

[ASheSChem]

Hi again,

maybe 20h-22h later, it's time to filtering

this is what it looks like... now i'm waiting for it to dry.

Thanks to all for helping, i'm happy

 

[ASheSChem]

and.. tadammm, the final product

but that smell like isopropanol... Air dry is so long.. beacause no vaccum pump ? any fast technic?

edit : and i have read somewhere the storage temperature for p2np is 2-8°C, you confirm that ?

 

[lazkalsai]

On the Internet you will mostly find to keep in cool 2-8°C dry and well ventilated place, but my friend kept his p2np in the frezzer (he had something like -15°C) and he has been using that and says that you can store it like that for pretty long time

 

[ASheSChem]

thanks,
do you know if i need a specific bottle or box palstic pe, pehd ... for long term storage?

 

[Mclssmxxl]

I keep mine airtight in the freezer, in the mylar(?) bag it came from the vendor, preferably not where the other reagents are.I stored it smelling a bit like isopropanol myself, it was fine weeks later, I just dried the amount I was working with by air before dissolving.

 

[ASheSChem]

thank you )

you think i can store it in a pharmatical glass amber bottle ?

 

[ASheSChem]

the end result is 43.5gr.
I think it's not much but I'm very happy about it and will do better next time.

Thanks again everyone <3

 

[ACAB]

The P2NP in a PP bag and this in a plastic container well closed and in the refrigerator, that should be for a while an usable pure product.

 

[ASheSChem]

Thanks

currently I do not use acetic acid. do you think i will have a better yeild by adding it to my recipe?

 

[Mclssmxxl]

Your reaction takes place at a sort of equilibrium, too complicated for me to understand for now, to explain i wont even try.But the takeaway is that if you start off with 50 molecules of your aldehyde + 50 of your amine the maximum yield with simple reflux is 50 molecules of propene + 50 of water.Because your reaction is then at equilibrium more of one of the products needs to be removed to push the eq in a way.Ideally if you remove the first 50 molecules of water that are formed, you esentially allow another 25 of water + 25 of propene to form.Removing another 25 allows another 12,5 to be formed and so on.

 

[ASheSChem]

i try to understand.. but maybe i'm too noob lol; but thanks for trying

 

[Mclssmxxl]

Here,

, jb will explain better.

 

[ASheSChem]

other topics..

last night, I put my pyrex dish (from yesterday synthesis) to dry in my incubator (DIY mushroom old stuff) an this morning, it's ultra dry, like rock of p2np

but.. it's perfect or it's too much?

Spoiler: photo

 

[Mclssmxxl]

Looks tasty now

 

[ASheSChem]

Thank you all for your help and support;
Before finishing with this this topic, I wanted to leave my conclusion there.

After 9 trying; it works without acetic acid but 20% less profitable. Acetic acid at 80° with a little isopropanol gives +-10% more.
The best is glacial acetic acid!

the best mix I tested was:
110gr benzaldehyde
80gr nitroethane
25ml glacial acetic acid
20ml cyclohexalamine

with a reflux of 3h30. 80% yield.

a little photo of pretty crystals to finish...

 

[MadHatter]

Thank you so much for this brilliant write-up and for your honest and hard-working experimentation! You have my utmost respect.

 

[KokosDreams]

Can the P2NP also be stored at negative degrees in a freezer?

@G.Patton

 

[G.Patton]

sure

 

[KokosDreams]

Amazing, thanks for reassuring