Question regarding amphetamine synthesis via P2NP + NabH4/CuCL2

[KokosDreams]

Hey folks,

going through my notes (read below) I am wondering about three main questions right now:


My questions now are:

1. What PH do I need to bring the reaction to before adding DCM?
2. Is it necessary to extract the aqueous phase with IPA or can I just extract with DCM and distill after adding NaOH at the end?
3. Is a 25% NaOH solution the best take or would another percentage of NaOH work better?
4. Instead of mixing the oil with water to prepare it for a steam distillation, can I fullfil a vacuum distillation in a rotavap too?

I was talking about the reaction with a friend and we got confused with these two steps

PS - This route was originally posted by @btcboss2022 and @William Dampier

Cincerly,

Koko

 

[Curiousonion]

Apparently IPA is not miscible with the salts so it will in fact separate.

 

[KokosDreams]

Yeah, I got very confused by our prior conversation. Great that we could solve it

 

[KokosDreams]

Did you found some more info on the PH, is it 11 like we already assumed?

Question no. 4 is solved, vacuum distillation will work better as we discussed yesterday.

Regarding Q3, what's your take on that? I've texted with others that use a lower concentration while others just use 25%, I lack understanding of why that is.

 

[Curiousonion]

No idea about the pH. None of the rxn mention it. Need to keep looking for that

 

[KokosDreams]

Gotcha!

 

[Curiousonion]

add cold saturated NaOH solution you made until you get to ~pH 11

 

[KokosDreams]

Perfect! What temperature is best for the 'cold' NaOH solution?

 

[Curiousonion]

Just keep the solution in the fridge

 

[KokosDreams]

Perfect, thanks for everything

 

[lisaalexander5478]

Great, what temperature is best ?