Problems with synthesis of amphetamine phosphate from P2NP via Al/Hg

[Mohammed_Lee]

I did so and with consultation from "the money" I came to better results. Now I'm optimizing my technique while waiting for the results of analysis. Here's a summery of my next tries:
The chemicals I used:

Al Foil (I don't know how many um but the premium one from Supermarket, thicker than the cheap ones) cut in stripes of about 0.5x5 cm
HAc 98%
IPA 99,9% (according to the label but when I tried to dry it with Natriumsulfate I noticed that it contains pretty much water) I Used it thuogh because I thought it goes in the RM that contains Water anyway.
NaOH p.A.
H3PO4 p.A.
Aceton Ph.Eur (water-free)

next try:

The main reaction with cooling was over after 10-15 min, the RM stood still 20 mins (under reflux) with a temperature of about 40°C. After 1:30 hours I transferred it to a beaker through a sieve and used a little bit of IPA to wash remainings from the round flask to the beaker. Then I added concentrated NaOH Solution in small portions until I reached a pH of about 11. The Solution stands still since about 6 hours and something was different this time. The two layers separated pretty fast I had different colors from what I had before.The bottom layer was almost black and the upper one has a yellowish/brown colour. The reaction was over faster because I couldn't see any bubbles after 3h. The bottom layer is about 210 ml and the upper one 130 ml.
I acidified in two parts: one with H2SO4/acetone 1:4 and the other one with H3PO4 (undiluted). The first half was yellowish before washing it with Acton and in the end I got about 2.5 g.
After letting the second part evaporating at 40°C the product was Pink/Red which I don't understand since I added the acid drop wise and when I got near 7 extra careful and slow. When it has reached about 7 I let it rest for 20 min with occasional stiring before adding the last drops. because pH paper isn't that accurate I stopped when it showed something between 6 and 7.

The next batch is evaporating right now and I got some questions left:

I want to keep the acetone dry so I stored a small part of it over a Molecular sieve 3A. It gets light yellow (because of "dust" from the molecular sieve I guess) how do I prevent this?

Is there any other method than simply adding the H3PO4 until reaching the desired pH and then evaporate the whole mixture? I can't find much about it here so if someone has experience or sources please let me know.

best regards,
Lee

 

[Mohammed_Lee]

Did you also have problems with over acidifying the base. I just evaporated the next batch and again: I stopped adding H2PO4 when I was more on the pH 7 than 6 range and the batch got pink/red after drying.
Is it possible that it has something to do with the evaporation process, should I add acid till I reached pH 8 or 9, evaporate half of the liquid and then check pH again?

 

[HairyPoppins]

we have all probably been thru the exact same thing. lol just get that top part and have fun! get the water out!

 

[ASheSChem]

Personnellement la seul fois où j'ai essayé avec de l'acide phosphorique, je n'ai pas eu de réaction non plus...

Alors qu'avec le même produit et de l'acide sulfurique, j'ai de très bon résultat ...

Du coup j'ai laissé tombé le phosphorique :x

 

[Chemdogkm]

The amine just weighs 10x the amount it actually is. Like if u put what a gram would be on the scale it will say 10 grams. 1g=10g. Idk y. Mines the same, but that is correct. Make hcl instead and burn sum on foil to make sure it is clean and correct.

 

[w2x3f5]

I received phosphate by dissolving a free base in dry acetone and slow adding phosphoric acid to ph 6, if ph goes below then the product of the snot

 

[HairyPoppins]

check ph

 

[Chemdog010297]

The amine salt just weighs different than usual weights of drugs. Like u said about 10x the regular amount. So 1g will say 10g.