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

[Mohammed_Lee]

Hello,

as I already described in another thread I got problems with the synthesis of amphetamine phosphate from P2NP via Al/Hg. I already made two Batches withe the same result: a much to high yield of whatever anorganic salts (for example 85g from 10g of P2NP). I followed every step from the Videos from this site and read about every thread in this forum and also a few other howtos. I alkanised my last batch about 14h ago and this is how it looks now

http://dumpliwoard5qsrrsroni7bdiishealhky4snigbzfmzcquwo3kml4id.onion/image/0275c4f5b897507c.jpeg

I somehow got three layers. the middle one looks like the upper one of my first 2 batches, I dont know why I got a third one.
Does anyone know what may went wrong with the first two batches, which mistake could have caused the results i got? What shell I do with this batch? Decant only the first layer, decant the first two or decant both in 2 different beakers?

I'm glad for any imput, thanks in advance,

lee

 

[Mohammed_Lee]

Update: I decided to put the middle and upper layer in a separatory funnel drained the middle layer back to the beaker and added phosphoric acid but no salt fell out (even after I added enough to reach pH 3).

 

[the money]

? to reply ?

 

[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?

 

[Mohammed_Lee]

Something strange happened during Washing. I added about 4 times the Volume of Aceton and got a deep Orange upper layer. I measured pH again and it still was somewhere between 6-7 after adding a drop of 1:1 Aceton H3PO4 it went to 6.
I transferred the upper layer into another beaker, added a few drops of acid/aceton mixture and some more salt fell out.
So I guess I made a mistake in another stage of the synthesis.

 

[UWe9o12jkied91d]

Perhaps you're not basifying sufficiently before dillution?
Red color is indicative of over-acid, it should be done slow and stirred well before taking measurement.

 

[DerBratling]

@Mohammed_Lee

Bro, what color was the stuff that floated on the surface when basifying to pH 12?
A basic rule of chemistry is: if you put shit in a reaction, you'll end up with shit.

 

[w2x3f5]

you produce sodium phosphate or sulfate on a good scale. At the end you have a solution of alcohol with a free amine base and a large amount of water, and in this mixture we will very well dissolve sodium hydroxide, which you then acidify with sulfuric or phosphoric acid. Overall your work is terrible.

 

[Manisj@1290]

Any One Help me

I tried to make Amphetamine. I cut 6 grams of aluminum foil into small pieces and put them in a 2L flask, then mixed some mercury nitrite, then 200 ml water. After some time, smoke started coming out from the mixture and the water became a little black, I washed it with water 3 times.

Then I mixed 5 grams of P2NP in 50 ml of Isopropanol Alcohol and 50 ml of water and heated it, when all the P2NP dissolved, then I mixed 25 ml of glacial acetic acid and put it in the same flask with Aluminum amalgam, but there was no exothermic reaction there. Well, after about 20 minutes very few bubbles are visible.
the aluminum foil was dissolving very slowly in the reaction, after 3-5 hours when all the aluminum foil was dissolved, I got a black colored solution mixture.

Then I prepared a solution of Sodium hydroxide and after it cooled, I added it to the solution and the reaction started, I saw 2 layers there, I separated the upper layer,
After that, I prepared a solution of 10 ml Acetone and 1 ml Sulfuric acid, and mixed it in a separate Amphetamine free base. When the pH of the paper became neutral, I stopped adding the solution of Sulfuric acid and Acetone in Amphetamine free base, in got some precipitation .that I had get Amphetamine in very small quantities, approximately 1.5 grams
Then I kept it at some distance from the burning bulb to dry. After a few hours, the amphetamine dried, then I wrapped it in a paper and when I looked again after a few hour, the amphetamine had again become a little wet and the quantity I got less
Then I gave a small dose of 20-25 mg to a man and he had a mild fever and was a little dizzy. And it's nothing like the pleasure or excitement you feel after taking amphetamines.

Can you tell me what mistake I made and why it is not working?

 

[w2x3f5]

Most likely there is a lack of mercury salt or the foil is dirty, the top layer after adding alkali was yellow-red in color? you got sodium sulfate mixed with amphetamine, which is why it turns damp in the air.

 

[Manisj@1290]

After adding the alkaline the amphetamine free base colour was slightly red. how to avoid moisture from Amphetamine salt

 

[w2x3f5]

problem with Al\Hg

 

[w2x3f5]

A good ratio for 1 gram of propene is to take 15 ml of isopropyl alcohol, 9 ml of acetic acid (98 percent) and 5 ml of water, 1.2 grams of foil (50 microns thick) + 75 milligrams of mercury nitrate. With proper operation, the output will be about 80 percent of the substance free of sodium sulfate impurities.

 

[HIGGS BOSSON]

The layer you need is the upper one, light yellow.
Does sulfate precipitate normally when sulfuric acid is added?
When oxidized with phosphate, flakes do not form immediately, they need to be acidified to neutral, and put to evaporate in a warm place for crystallization.
Many young chemists are interested in phosphate, because in some cases it is easier to buy orthophosphoric acid than sulfuric acid. And I personally like the effect of amphetamine phosphate more - a softer effect.
We will make a video on the topic of obtaining different amphetamine salts for the BB community.