Amphetamine Reagent Kit

[JohnWebb]

Amphetamine Synthesis Report​

First of all I would like to thanks to @William Dampier & @Marvin "Popcorn" Sutton for synthesis kit, mentoring and help.
Thank you very much experts ! ​

1. 12g of aluminium foil was cutted and then shredded into 0,8mm strips. The strips were a bit wrinkled so I straightened them all with gloves and then placed into flask.

2. Prepare the alkaline solution.​

- Next I made NaOh solution (50g per 70ml) and put aside.

3. Preparation of phenylnitropropene solution​

- I prepared solution of 100ml IPA, 20ml water and 10g P2NP.
I heated it up, dissoluted it while stirring and set it aside to cool.

4. Amalgam​

- I covered cutted aluminum foil in a flask with distilled water.
The foil layar was completely hidden under water.
Added 0,1g of Mercury Nitrate into flask and stirred by circular motions.

Meanwhile I added 50ml of GAA into P2NP solution from step 3. which I heated for a while beforehand to dissolve the crystals that
formed.

When water turned into gray color I drained water out with sieve.
I quickly washed the foil twice with distilled water.

5. Synthesis of amphetamine​

- I added in 2 portions p2np solution into flask with amalgam and put on the reflux consender. Stirring it with gentle circular motion.

If the flask was burning my bare hand holding it from below, I put it in a container of cold water to cool the temperature.

After the boisterous part of the reaction has passed, I let it rest for 30 minutes until the flask showed no signs of reaction.

6. Alkalinization and extraction of free amphetamine base​

- I poured reaction mixture into beaker through a sieve. There was a lot of foil left in the sieve.

I added with stirring NaOH solution in portions to pH11.

After about 20h I collected top layer.

7. Acidification​

- Added 10ml acetone to 1 ml of concentrated sulfuric acid and stirred. Then I carefully added drop by drop to the yellow layer from the previous steps until pH 6. After acidification I placed mixture in the freezer over night.
Next day i filtered this white paste in a buchner funnel under vacuum.
After the first filtration I disluted amphetamine with a small portion of acetone and then filtered again and put it to dry.

I'm currently solving yieldings problems. I will update soon.

 

[Djdrama]

What is the yield brother?
Because you didn't reflux it.
I lent that you can lost 20% of products if you didn't reflux for 30 yo 60 minutes.
Products can also be lost in the unrelated aluminium foil.

 

[JohnWebb]

What is the yield brother?
Because you didn't reflux it.
I lent that you can lost 20% of products if you didn't reflux for 30 yo 60 minutes.
Products can also be lost in the unrelated aluminium foil.

DjdramaThank you for your advice - exactly as you write, the yield from this attempt was only 5,5g so about 20% less than it should be.
The experts have advised me to do exactly that, I'll give it a try and update the thread soon.

 

[anonimxx99]

6. Alkalinization and extraction of free amphetamine base
- I poured reaction mixture into beaker through a sieve. There was a lot of foil left in the sieve.

did the layers separate on their own or did you add something to the mixture?

 

[ENZO]

6. Alkalinization and extraction of free amphetamine base
- I poured reaction mixture into beaker through a sieve. There was a lot of foil left in the sieve.

did the layers separate on their own or did you add something to the mixture?

View attachment 24808

anonimxx99I think at this point you should alkalize with the NaOH solution.

 

[JohnWebb]

I think at this point you should alkalize with the NaOH solution.

ENZOYeah, I added with stirring NaOH solution in portions to pH11.
Apparently I must have accidentally removed this step when uploading the images. Thank you @anonimxx99

 

[anonimxx99]

Yeah, I added with stirring NaOH solution in portions to pH11.
Apparently I must have accidentally removed this step when uploading the images. Thank you @anonimxx99

JohnWebbok, thanks, and tell me, do I have to wait 20 hours before acidifying?

 

[anonimxx99]

Yeah, I added with stirring NaOH solution in portions to pH11.
Apparently I must have accidentally removed this step when uploading the images. Thank you @anonimxx99

JohnWebbWhich naoh solution did you add warm or cold?

 

[ENZO]

Can this method be modified to use P2P instead of P2nP?

 

[hoboking]

judging from the pictures it looks like you had very weak/incomplete al/hg reaction,in order to get good yield/good product you need to have strong reaction.did you get the "kickoff" you know when the reaction starts it goes like swooosh and the pressure starts to coming out of the condenser and the reaction starts to boil and foam like crazy?