One-pot Amphetamine Synthesis From P2NP With NaBH4/CuCl2 (1kg scale)

[diogenes]

I think this has got to do with the pKa of the amphetamine base, which is around 9-9.5 if I remember well.

 

[guero1k]

What is the cost of producing a kilogram of finished ice?.... Using this method of course.

 

[WinterDust]

Hi,

Posts like these just bums me out.

You register at a forum, do one login and ask a question within a second without doing the slightest research.

You don't deserve an answer since it actually already is answered in the forum.

 

[WinterDust]

Hi,

So I did my little experiment, regarding the synthesis.

This was my measurements:

IPA/H20 2:1 - 3,6L
NaBH4 - 348G
P2nP - 480G (Increased from 200G)
CuCl2 - 40G
NaOH 25% - 1,6L

This is the result from my synthesis and tripple filtration.

If you look at my previous synthesis (200g P2nP) the amphetamineoil was bright yellow.

This amphetamineoil (480g P2nP) is dark orange, looks very good to me.

Tomorrow I will find out what the final yield will be from this reaction and I will update with results.

 

[WinterDust]

Conclusion to my little experiment.

Don't do it

 

[Fenster]

4

 

[Bartholomeus]

The color of your finished reaction looks like some p2np hadn't been reacted fully
So what did you get out of it?

 

[WinterDust]

That may be true, 1 1/2h into the process, the reaction kind of stopped and the temperature only decreased.

Once I poured the CuCl2 into the mix it only changed color, and it was a b*tch to keep the temperature at 80C in the end but I managed.

I started the crystalization with the sulfuric acid, but the problem was that the pH sticks kept the same color as the amphetamine oil, dark orange, didnt matter how much I poured inside, so in the end I gave up and discharged of it all.

It is not worth all of the hastle just to save up on some IPA and NaBH4.

 

[Bartholomeus]

Thanks for the update, may I ask you what is your flask size? 5L?
What is your yield of dry sulphate from your previous 200g p2np reactions?

 

[G.Patton]

Have you checked boiling temperature of your "amphetamine base"? It looks like not amphetamine oil. Have you got any sediment after H2SO4 solution addition?

 

[WinterDust]

No, I did not check the boiling temperature of the amphetamine base.

Well, it was amphetamineoil since it actually did crystalize during sulfuric acid process, my only problem was that I could not see the value of the pH sticks because of the discoloration of the oil, it got very very dark orange once I started to ad sulfuric acid, so my best guess would be, one would need to use a digital pH meter to determine.

I go amphetamineoil > filtration > crystalization > vacuum.

 

[WinterDust]

I use a 10L flat bottom florence flask, I works perfectly with my reaction scale.

My yield so far has been 90% and I'm very happy with this.

 

[G.Patton]

Hmm, you told that you add sulfuric acid and don't use H2SO4 I'm a little bit confused. You also can steam distill amph free base to get pure oil.

 

[WinterDust]

My bad, I was all up in my head, I answered wrongfully, it has been edited.

Yes, I know, I tried building a distillation attraption, but there are to many joints to grease with vacuum grease and keep track of pressure etc. and I don't see the use to buy a rotovap.

You can just aswell just crystalise the product straight after adding the NoAH 25%, this is what I do. I also sent my amphetamine for analysis and it came back 90-95% pure.

 

[Bartholomeus]

Thanks for answer, do you use condenser on top of reaction? You take it off when you add p2np portion wise?
And what is your temperature when you add cucl2 to reaction? Do you heat reaction after the p2np addition is finished and then add cucl2
or when the p2np addition is finished you just add cucl2 and then heat the reaction to boil for half hour?
Please explain your process a bit as I am interested to know how you achieve such high yield

 

[Bartholomeus]

Hi mate did you try this reaction in Methanol maybe also?

 

[WinterDust]

To be honest with you, I just follow the "recipe" to a T and use graded equipement.

If you do just as it is written you'll make the same progress.

 

[KokosDreams]

What cooling system do you use for your 10L flask?

 

[WinterDust]

Hard question to answer, since I built my own cooling system.

 

[ElementalEnigma]

What did you use for a cooling system?

 

[KokosDreams]

That's what I thought.

Could you describe that to me? That's the big question mark I still got. As my lab equipment is already ordered and I'll be ready to start soon, I would like to solve this issue before