P2P Synthesis From P2NP

[K-Cyanide]

No, absolutely in the sense, the reaction won´t work using undistilled P2P, is it not.
However, the final product is always of higher quality when you use distilled compounds. And not to forget, dirty P2P hurts the yield, no doubt. Its a tedious work, but it pays off.

 

[Multivitamin]

Okay will distill it.Guess no way around it.Do you think that it is absolutely necessary to measure pressure in in system when vacuum distilling p2p oil/meth freebase oil?Or can i just plug-in vacuum pump to vacuum adapter on new empty receiving flask when DCM has been distilled off (cause DCM with low boiling bp. of 50c would distill even without vacuum) turn on the vacuum crank up the heat until i see first signs of p2p oil coming over to receiving flask and hold temperature until distillation is over.

Am i missing something here?Do i have to measure that pressure of the vacuum?Or can i just slowly crank the heat up until i see oil coming over in receiving flask?

 

[G.Patton]

Read about Distillation and distillation systems, it would be very helpful for you.

 

[Cardboard1234]

Hey guys, after adding DCM and washing with NaOH, my bottom layer is green instead of red like in the video. I am gonna distill this and see if I can get any P2P but has anyone experienced a similar issue as this? Why is the colour different?

 

[G.Patton]

How can we answer you without any input data about your reagent/synthesis manipulations? Distill it and then check bp or/and refraction index.

 

[Cardboard1234]

Hey Patton, sorry for the lack of information. I’ll be more specific here.

I followed the steps exactly as shown in the video for this synthesis except I wasn’t able to bring the temperature down to 0-5deg Celsius on the NaBH4 addition step.

I also did not add HCl in a drop wise manner but I added it in 100ml successions.

I have successfully distilled the DCM in the mixture as it was lingering around 80deg C, after that it went beyond 80 deg C and I started noticing a transparent layer above my DCM that isn’t soluble with DCM. I’m guessing it’s water,

I am currently boiling the Rm further and I am currently seeing a light yellow solution in my receiving flask and my thermometer is showing 220 deg C.

This looks like P2P

 

[G.Patton]

So, what is a problem? =)

 

[Cardboard1234]

I’m not too sure if it is P2P as I read in one of your threads that we are not allowed to pour in HCl without being drop wise as it will spoil our product and I’m not sure if exceeding the specified temperature would give me a different product as well.
How would I know if it’s pure P2P now?

 

[Cardboard1234]

The temperature exceeded 220 and hit 280 at one point and now my receiving flask has two layers. Not sure what I’m looking at now too

 

[G.Patton]

Yes, it can spoil your product completely. You can check its boiling point by distillation method.

 

[K-Cyanide]

You must not heat P2P to 220C, at these temperatures you ruin the molecule as it decomposes. Obtaining pure P2P via distillation has to be accomplished under reduced pressure (aka vacuum distillation). You can determine the boiling point of your P2P when you have calibrated you vacuum source. With an aspirator water pump with common water pressure (ca. 3.5 bat) P2P boils appr. at 105C.
Beside the boiling point you can determine the density (almost equal to water) and the colour/smell. Pure P2P is clear to pale yellow and has a pleasant flowery smell.

 

[K-Cyanide]

oh sorry did not want to reply to you G.Patton.

 

[Cardboard1234]

Hey thanks @K-Cyanide, I was still thinking if I could still save my solution but it looks like it's completely decomposed as it is now completely black. I am now looking for a vacuum distillation set to achieve this. Is there any that you would recommend? I'm not too sure how to calibrate our vacuum source but I'll look into it, do you have any sources I could look into on this? Thank you so much for your response!

 

[K-Cyanide]

@Cardboard1234[/USER] you are welcome. I am glad to help and I am happy there is such a great forum which brings warm memories of the legendary Hive forum to me. Back to the topic:
To determine the strength of the vacuum connect a small RBF (250 or 500ml) to your vacuum source and fill it with a quarter or third of water. Then apply full blast vacuum. Then observe whether the water in the flask starts to boil or not.
This should also be done in a certain time period (depending on the size of the flask i.e. 250ml under 30 seconds), this ensures your vacuum source provides a sufficient volume flow.
The alternative is a chemical resistant diaphragm pump (Vacuubrand, KNF, IKA, Edwards etc. With a little patience you will find good used pumps on Ebay for a couple of hundred Dollars/Euros.

 

[curiousmind]

The video says to add acid until a pH of 5-4 or less yet the write up says 6.5- 7. Can someone please clarify what the correct pH should be please

 

[madafaka]

So i was following the protocol and was adding acid dropwise until ph 6 -7 layers have separated in to two distinct layers like you see on the photo, but when adding DCM i could not clearly see the dcm layer.They are still only two layers.

This photo of the reaction flask is just reaction mixture, this other photo of the rm in the beaker is with added DCM

I will give 500 usd in bitcoins to anyone who will help me to get trough this.

 

[T 3]

Think your product now in your lower layer

 

[Czeczeczecze]

I can't obtain h2o2 in 30% concentration. Can I use 12% in bigger quantity? or what can i use instead off h2o2?

 

[PolandoEmingarnte]

because in poland is illigal 30%

 

[amieri]

You concentrate it by evaporating the water out of it.

 

[Zhopkins05]

Can anyone help in my last step washing the dcm with NoAH my product went into the aqueous layer and left my dcm green

 

[T 3]

What was or is your ph , how concentrated was ur NaOH

 

[Zhopkins05]

Ph was about a 4 I kept adding the acid but it didn’t go up anymore stayed at 4 and 25% with the extra H20