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

[HEISENBERG]

@HEISENBERG

Could you please add this one to the sticky posts?

KokosDreamsDone

 

[KokosDreams]

Done

HEISENBERGThanks

 

[diogenes]

Hi,

I have just done this synthesis and the yield is 60%+ (some acetone still in the freezer), which is not bad considering that at some point the reaction mass spillt out (overheated and started to expand). I quickly cooled it and then kept a reflux condenser on top for the rest of the reaction (the original description does not mention this). There is some delay in the heat increase following the addition of a portion of the P2NP, which needs to be considered, I added a further portion too quickly. A cold bath is handy. The endproduct is very efficient in terms of bio-test, I am doing an acid-base extraction to see whether there are other chemicals is the endproduct as well. There is a slight, distinct smell, which I identify as close to the smell of Cu perhaps?, which lingers despite 5X Acetone wash and having a very white, pure looking product.

I was wondering if there is anyone here, who could write out the exact reaction what is happening in this synthesis. The role of CuCl2 is not clear to me and also how the H atoms move etc. It would be very useful to have the reaction explained in a bit more detail. Apologies, if this has already mentioned, I have seen most of this thread, but haven`t had the chance to catch up lately. Thank you

 

[WinterDust]

Hi,

How is this reaction scaled, is it linear?

I would appreciate help with scaling appropriate for a 10L round bottom flask and a 20L round bottom flask.

Best Regards

 

[G.Patton]

Hi,

How is this reaction scaled, is it linear?

I would appreciate help with scaling appropriate for a 10L round bottom flask and a 20L round bottom flask.

Best Regards

eyelowYes, it is possible.

 

[diogenes]

How is this reaction scaled, is it linear?

I would appreciate help with scaling appropriate for a 10L round bottom flask and a 20L round bottom flask.

Best Regards

eyelow
I forgot to mention in my post that I heavily scaled down the synthesis, using only 25g of P2NP. I simply divided everyting by 1000/25=40 and used a 2l flask. Although the amount was less than half of the flask I still managed to spill some so I would suggest using a reflux by default to prevent this or just keep in mind that following the addition of a portion of P2NP there is a time-lag until it starts reacting so the addition should be real slow and gradual. This is definitely what I`m going to use next time. The other change I did was to reduce the amount of solvent in the end (not until only oil was left) and then precipitate by IPA-Sulphuric acid (10-1) until Ph 6-7.

 

[Bartholomeus]

Obtained yield from 100g P2NP as starting material was 78g pure white dried sulfate
Used was IPA/water in 2:1 ratio like in original synthesis (1200ml IPA / 600ml Water)
150g NaBH4, added in 2 portions, first portion 100g at the start mixed with ipa and water
Then after all the p2np has been added (when adding p2np use cold water for cooling the vessel)
Then added 50g NaBH4 again to vessel, and proceeded to heat the mixture to 50 degrees
and when the reaction was hot in one portion added 30g of CuCL2 (CuCl2 was dissolved in 100ml IPA / 50ml water)
Addition produced volcano style eruption which blew a bit of CuCl2 out of vessel - but not a problem
After this step, reaction was heated to a boil for good 45 minutes, after it was basified with NaOH and separated the top layer
Which was IPA with freebase
Water cooled condenser on vessel has been used from start to finish, otherwise you will lose too much solvent

And I also can confirm the smell you @diogenes are experiencing, the same weird smell after Cu - even after numerous IPA cleanings of product
Maybe after few days outside it will subside

Nevertheless this reaction is one of the most cleanest and simplest reactions ever done in one pot

 

[diogenes]

Obtained yield from 100g P2NP as starting material was 78g pure white dried sulfate
Used was IPA/water in 2:1 ratio like in original synthesis (1200ml IPA / 600ml Water)
150g NaBH4, added in 2 portions, first portion 100g at the start mixed with ipa and water
Then after all the p2np has been added (when adding p2np use cold water for cooling the vessel)
Then added 50g NaBH4 again to vessel, and proceeded to heat the mixture to 50 degrees
and when the reaction was hot in one portion added 30g of CuCL2 (CuCl2 was dissolved in 100ml IPA / 50ml water)
Addition produced volcano style eruption which blew a bit of CuCl2 out of vessel - but not a problem
After this step, reaction was heated to a boil for good 45 minutes, after it was basified with NaOH and separated the top layer
Which was IPA with freebase
Water cooled condenser on vessel has been used from start to finish, otherwise you will lose too much solvent

And I also can confirm the smell you @diogenes are experiencing, the same weird smell after Cu - even after numerous IPA cleanings of product
Maybe after few days outside it will subside

Nevertheless this reaction is one of the most cleanest and simplest reactions ever done in one pot

ChingShihWhy did you add so much CuCl2? I was thinking that the weird smell might be due to impurities in my CuCl2 (which I prepared from some copper pipes), but if you had the same it means there might be some Cu or Cu related impurities in the product. By the way, I did an acid base extraction on some portion of the yield and the smell completely disappeared.

 

[KokosDreams]

Obtained yield from 100g P2NP as starting material was 78g pure white dried sulfate
Used was IPA/water in 2:1 ratio like in original synthesis (1200ml IPA / 600ml Water)
150g NaBH4, added in 2 portions, first portion 100g at the start mixed with ipa and water
Then after all the p2np has been added (when adding p2np use cold water for cooling the vessel)
Then added 50g NaBH4 again to vessel, and proceeded to heat the mixture to 50 degrees
and when the reaction was hot in one portion added 30g of CuCL2 (CuCl2 was dissolved in 100ml IPA / 50ml water)
Addition produced volcano style eruption which blew a bit of CuCl2 out of vessel - but not a problem
After this step, reaction was heated to a boil for good 45 minutes, after it was basified with NaOH and separated the top layer
Which was IPA with freebase
Water cooled condenser on vessel has been used from start to finish, otherwise you will lose too much solvent

And I also can confirm the smell you @diogenes are experiencing, the same weird smell after Cu - even after numerous IPA cleanings of product
Maybe after few days outside it will subside

Nevertheless this reaction is one of the most cleanest and simplest reactions ever done in one pot

ChingShihThanks for contributing this

 

[diogenes]

This reaction is very good on a small scale
In a large reaction, trying to control the exotherm and the large amount of foam by putting the CuCl2 solution slowly into the flask will not give a high yield, there may be nothing but nitroalkanes and the concentration of nanoparticles will be too small to reduce the nitro, the largest flask possible should be used and the entire CuCl2 solution should be added at once

Uncle LeeUncle Lee, I have just realised that you said some very important things which I don`t fully understand. What do you mean by nanoparticles? In general I don`t understand the role of CuCl2 in the reaction, can you please explain this and also the nanoparticles part? Apologies for the delayed reaction to your post.

 

[Bartholomeus]

Why did you add so much CuCl2? I was thinking that the weird smell might be due to impurities in my CuCl2 (which I prepared from some copper pipes), but if you had the same it means there might be some Cu or Cu related impurities in the product. By the way, I did an acid base extraction on some portion of the yield and the smell completely disappeared.

diogenes
My CuCl2 was chemical purity 99.8%, I added it because it couldn't hurt the reaction because of it and one of the Forum Experts proposed even higher Cucl2 ratio...

 

[Mo0odi]

Is there a synthesis of CuCl2

 

[Mo0odi]

A NaOH (8 liters 25%) water solution of is added to the reaction mixture and layers are separated.

After dozens of successful syntheses, it actually failed for me this time.
my glass reactor had a small crack which unfortunately led to a large one and has therefore become leaky. Luckily this happened shortly before the addition of CuCl2. I then stopped the synthesis, quenched the reaction with H2o and put it in a canister.
My question now: Can the mixture of NabH4 and P2NP be separated in any way so that both can be returned to their original forms? so that it can be used again for another new synthesis.

Sasha89I have sodium hydroxide granules, how do I make them 25% solution ?

 

[diogenes]

Is there a synthesis of CuCl2

Mo0odiYou can find plenty of videos on youtube. Basically find some pure copper (e.g. wires etc.) then add some HCl and H2O2. If your hydrogen peroxide is strong then add it very carefully as the reaction can be quite stormy.

I have sodium hydroxide granules, how do I make them 25% solution ?

1 liter of distilled water + 250g of NaOH. It refers to the weight percentage and 1l of water is 1000g.

 

[Curiousonion]

I thought 25% solution means 250 grams NaOH in 750ml of water no?
I read some say 25 grams in 75 ml and some say 25 grams in 100ml.

 

[Curiousonion]

20% NaOH (W/V), means 20 grams of NaOH solids, dissolved in distilled water until you have 100mL of aqueous solution. Do this in beaker slowly, and drip water until it reaches exactly 100 mL mark. 20% NaOH(W/W) means 20 grams of NaOH solids plus 80 grams of distilled water, making up 100 grams of solution.

 

[KokosDreams]

I thought 25% solution means 250 grams NaOH in 750ml of water no?
I read some say 25 grams in 75 ml and some say 25 grams in 100ml.

CuriousonionYes because 25gr in 100ml/ would be a 20% NaOH solution, not 25%

 

[Curiousonion]

Yup, 25/125 is 20%.

Yes because 25gr in 100ml/ would be a 20% NaOH solution, not 25%

KokosDreams

 

[Mo0odi]

Thanks everyone for sharing

 

[WinterDust]

So, I started my first synthesis today, did not go very well.

The reaction at higher volumes is VERY exothermic (200g P2nP) and just as previous poster stated, it's a very delayed reaction.

I used a 10l roundbottomflask with a 400mm cooler, unfortunetly I added too much P2nP at once (100G) and the cooler broke of accidently, so I had a 1m (3foot) volcano in my house ..

Well, spent 2 hours cleaning everything when everything calmed down and I ventilated the whole room.

So lesson, there is a delayed reaction when adding the P2nP so poor very gently and wait, secondly be vary of a good chilled cooler connected.

I'll do my second attempt tomorrow or the day after.

I'll keep people posted, best regards.