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



## ASheSChem

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



> 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.
> 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.
> 50mL of H2O were added and then sucked off with a pipette until the phenyl-2-nitropropene crystallized (it crystallized when it came in contact with air in presence of 15mL H2O).
> I added 200mL 95% denaturated ethanol to the orange crystals.
> The color of the now needle-like crystals changed from orange to white-yellow. The crystals were filtered. Yield 65 g, 78% of theory.





> To 55 g (0.5mol) Benzaldehyde in a 500mL Flask were added 40 g (0.5mol) Nitroethane and 10mL Cyclohexylamine.


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



> The result 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.


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



> 50mL of H2O were added and then sucked off with a pipette until the phenyl-2-nitropropene crystallized (it crystallized when it came in contact with air in presence of 15mL H2O).


So.. it cristalized in the flask with all liquids (and no need freeze or something like that..?)


> I added 200mL 95% denaturated ethanol to the orange crystals.


We don't need to filter the crystals before add the ethanol ?

that's it... Thank youuu


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## HIGGS BOSSON

ASheSChem said:


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



ASheSChemIt 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.


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## ASheSChem

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


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## 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...


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## Mclssmxxl

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


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## 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?


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## 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.


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## G.Patton

ASheSChem said:


> any tips for a fast drying with no vaccum pump ?



ASheSChemHow 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


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## Honolulu98

ASheSChem said:


> 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.
> View attachment 4332View attachment 4333View attachment 4334
> 
> after that, cooling at room temperature...
> View attachment 4335
> 
> 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
> View attachment 4336
> 
> and i put it in the freezer... (actually 11h)
> View attachment 4337
> 
> to be continued...



ASheSChem
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


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## ASheSChem

Thanks all for good vibes




Mclssmxxl said:


> 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.



Mclssmxxlok 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 



G.Patton said:


> 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



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



Honolulu98 said:


> 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



thanks a lot, hope you the best


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## 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?


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## G.Patton

ASheSChem said:


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



ASheSChemyes


ASheSChem said:


> freezing?


No, you can get crystalline impurities after freezing.


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## 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


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## ASheSChem

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

I had to wait 24 hours?
big mistake?


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## William Dampier

ASheSChem said:


> oops... I just realized that I filtered directly after heating and mixing...
> 
> I had to wait 24 hours?
> big mistake?



ASheSChemNo, save the filtered liquid and let crystallize too.


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## 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


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## 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.


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## ASheSChem

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


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## 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.


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## 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...


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## HIGGS BOSSON

ASheSChem said:


> 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
> 
> 
> 
> View attachment 4387
> 
> 
> 
> I have to leave the flask open for evaporation for 24 hours or not?
> before filtering...



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


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## 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


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## 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 ?


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## 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


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## ASheSChem

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


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## 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.


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## ASheSChem

thank you )

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


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## 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


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## ACAB

ASheSChem said:


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



ASheSChem


ASheSChem said:


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


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.


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## ASheSChem

Thanks 

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


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## 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.


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## ASheSChem

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


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## Mclssmxxl

Here, 



, jb will explain better.


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## 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


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## Mclssmxxl

ASheSChem said:


> 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
> 
> 
> 
> View attachment 4624



ASheSChemLooks tasty now


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## 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...


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## MadHatter

ASheSChem said:


> 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...
> 
> View attachment 4751​



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


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## KokosDreams

ACAB said:


> 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.



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

@G.Patton


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## G.Patton

KokosDreams said:


> Can the P2NP also be stored at negative degrees in a freezer?
> 
> @G.Patton



KokosDreamssure


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## KokosDreams

G.Patton said:


> sure



G.Patton
Amazing, thanks for reassuring


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## 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!


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## Evilcarrot2




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## Evilcarrot2

Before put into desicator


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## 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.


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## Evilcarrot2

TotalSynthesis said:


> 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.



TotalSynthesisThanks 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


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## 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


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