Complete amphetamine freebase (A-oil) synthesis from P2P(10L scale)

[Davidrobinson]

Is that picture after internal steam distillation?
Did you distill your p2p for 70% yield , or did you use it straight from bmk ?

 

[blackburn]

Is that picture after internal steam distillation?
Did you distill your p2p for 70% yield , or did you use it straight from bmk ?

oscar412Yes it is .

I used The P2P immediately after conversion from 5449, i did not distill it.

 

[damakemi]

Yes it is .

I used The P2P immediately after conversion from 5449, i did not distill it.

blackburndid you wash the p2p?

 

[damakemi]

I added the 2 ways of N-Formylamphetamine Hydrolysis and as always is MY way and it works for ME don't means is the only and official way.

N-Formylamphetamine
​

1. Put 10L of P2P in the reactor, add 15L of formamide and 7L of formic acid, slow stirring with reflux during 5 hours at 140/150C.
2. Stop heating and cool it until a temp where you can add H2O without a big evaporation, add 13,33L of H2O mix and let separated the layers.
3. Keep the top layer(oil layer)
4. Bottom layer( water layer) is extracted with DCM, let the layers separate completely, add the bottom layer(DCM layer) to the layer kept in the point 3, mix them, dry it with anhydrous Na2SO4 or MgSO4, filter it and evaporate DCM.(Optional)
5. You should get around 11L of N-Formylamphetamine.

N-Formylamphetamine Hydrolysis by HCL way​

1. Put the 11L of N-Formylamphetamine in the reactor, add slowly 11L(1:1) of HCL 37%, slow stirring with reflux during 2 hours at 80/90C.
2. Stop heating and cool it until 25C, add 10L of DCM mix and let separated the layers.
3. Keep the top layer, bottom layer(DCM layer is discarded)
4. Add the cold top layer to a previous cold solution of 1,66kg of NaOH+ 2,66L of H20, let it cool at RT 12 hours.
5. 2 layers separated keep top layer(oil layer)
6. Bottom layer( water layer) is extracted with DCM, let the layers separate completely, add the bottom layer(DCM layer) to the layer kept in the point 5, mix them and evaporate DCM.(Optional)
7. The mixture is steam distilled at 140-145C to get a transparent oil, at 100C oil starts to run out in the cooler at 130C turn on the steam and don't heat it more than 150C in that case you will get yellow oil.
8. Let separate completely the 2 layers of your distillation receiving flask, keep the top layer(oil layer)
9. Bottom layer( water layer) is extracted with DCM, let the layers separate completely, add the bottom layer(DCM layer) to the layer kept in the point 8, mix them, dry it with anhydrous Na2SO4 or MgSO4, filter it and evaporate DCM.(Optional)
10. 8,3L of amphetamine freebase obtained.

N-Formylamphetamine Hydrolysis by NaOH way
​

1. Put the 11L of N-Formylamphetamine in the reactor, add 13L previous cold 65% NaOH solution slow stirring with reflux during 2-3 hours at 110C.
2. Stop heating and cool it at RT
3. Keep the top layer(oil layer)
4. Bottom layer( water layer) is extracted with DCM, let the layers separate completely, add the bottom layer(DCM layer) to the layer kept in the point 3, mix them and evaporate DCM.(Optional)
5. The mixture is steam distilled at 140-145C to get a transparent oil, at 100C oil starts to run out in the cooler at 130C turn on the steam and don't heat it more than 150C in that case you will get yellow oil.
6. Let separate completely the 2 layers of your distillation receiving flask, keep the top layer(oil layer)
7. Bottom layer( water layer) is extracted with DCM, let the layers separate completely, add the bottom layer(DCM layer) to the layer kept in the point 6, mix them, dry it with anhydrous Na2SO4 or MgSO4, filter it and evaporate DCM.(Optional)
8. 8,5L of amphetamine freebase obtained.

​

btcboss2022I did the Naoh way was wondering if it's possible to distill the oil right after 2-3 hours reflux, after point 2 ?

 

[btcboss2022]

I did the Naoh way was wondering if it's possible to distill the oil right after 2-3 hours reflux, after point 2 ?

damakemiSteam distillation yes.

 

[damakemi]

Steam distillation yes.

btcboss2022thanks for answering, can I make a larger amount of formamide and formic acid mix and store it?

 

[btcboss2022]

thanks for answering, can I make a larger amount of formamide and formic acid mix and store it?

damakemiwhat you mean exactly?

 

[MisterAnonymous]

I added the 2 ways of N-Formylamphetamine Hydrolysis and as always is MY way and it works for ME don't means is the only and official way.

N-Formylamphetamine
​

1. Put 10L of P2P in the reactor, add 15L of formamide and 7L of formic acid, slow stirring with reflux during 5 hours at 140/150C.
2. Stop heating and cool it until a temp where you can add H2O without a big evaporation, add 13,33L of H2O mix and let separated the layers.
3. Keep the top layer(oil layer)
4. Bottom layer( water layer) is extracted with DCM, let the layers separate completely, add the bottom layer(DCM layer) to the layer kept in the point 3, mix them, dry it with anhydrous Na2SO4 or MgSO4, filter it and evaporate DCM.(Optional)
5. You should get around 11L of N-Formylamphetamine.

N-Formylamphetamine Hydrolysis by HCL way​

1. Put the 11L of N-Formylamphetamine in the reactor, add slowly 11L(1:1) of HCL 37%, slow stirring with reflux during 2 hours at 80/90C.
2. Stop heating and cool it until 25C, add 10L of DCM mix and let separated the layers.
3. Keep the top layer, bottom layer(DCM layer is discarded)
4. Add the cold top layer to a previous cold solution of 1,66kg of NaOH+ 2,66L of H20, let it cool at RT 12 hours.
5. 2 layers separated keep top layer(oil layer)
6. Bottom layer( water layer) is extracted with DCM, let the layers separate completely, add the bottom layer(DCM layer) to the layer kept in the point 5, mix them and evaporate DCM.(Optional)
7. The mixture is steam distilled at 140-145C to get a transparent oil, at 100C oil starts to run out in the cooler at 130C turn on the steam and don't heat it more than 150C in that case you will get yellow oil.
8. Let separate completely the 2 layers of your distillation receiving flask, keep the top layer(oil layer)
9. Bottom layer( water layer) is extracted with DCM, let the layers separate completely, add the bottom layer(DCM layer) to the layer kept in the point 8, mix them, dry it with anhydrous Na2SO4 or MgSO4, filter it and evaporate DCM.(Optional)
10. 8,3L of amphetamine freebase obtained.

N-Formylamphetamine Hydrolysis by NaOH way
​

1. Put the 11L of N-Formylamphetamine in the reactor, add 13L previous cold 65% NaOH solution slow stirring with reflux during 2-3 hours at 110C.
2. Stop heating and cool it at RT
3. Keep the top layer(oil layer)
4. Bottom layer( water layer) is extracted with DCM, let the layers separate completely, add the bottom layer(DCM layer) to the layer kept in the point 3, mix them and evaporate DCM.(Optional)
5. The mixture is steam distilled at 140-145C to get a transparent oil, at 100C oil starts to run out in the cooler at 130C turn on the steam and don't heat it more than 150C in that case you will get yellow oil.
6. Let separate completely the 2 layers of your distillation receiving flask, keep the top layer(oil layer)
7. Bottom layer( water layer) is extracted with DCM, let the layers separate completely, add the bottom layer(DCM layer) to the layer kept in the point 6, mix them, dry it with anhydrous Na2SO4 or MgSO4, filter it and evaporate DCM.(Optional)
8. 8,5L of amphetamine freebase obtained.

​

btcboss2022

Thanks Maestro didn't get it at first now i do

 

[damakemi]

I added the 2 ways of N-Formylamphetamine Hydrolysis and as always is MY way and it works for ME don't means is the only and official way.

N-Formylamphetamine
​

1. Put 10L of P2P in the reactor, add 15L of formamide and 7L of formic acid, slow stirring with reflux during 5 hours at 140/150C.
2. Stop heating and cool it until a temp where you can add H2O without a big evaporation, add 13,33L of H2O mix and let separated the layers.
3. Keep the top layer(oil layer)
4. Bottom layer( water layer) is extracted with DCM, let the layers separate completely, add the bottom layer(DCM layer) to the layer kept in the point 3, mix them, dry it with anhydrous Na2SO4 or MgSO4, filter it and evaporate DCM.(Optional)
5. You should get around 11L of N-Formylamphetamine.

N-Formylamphetamine Hydrolysis by HCL way​

1. Put the 11L of N-Formylamphetamine in the reactor, add slowly 11L(1:1) of HCL 37%, slow stirring with reflux during 2 hours at 80/90C.
2. Stop heating and cool it until 25C, add 10L of DCM mix and let separated the layers.
3. Keep the top layer, bottom layer(DCM layer is discarded)
4. Add the cold top layer to a previous cold solution of 1,66kg of NaOH+ 2,66L of H20, let it cool at RT 12 hours.
5. 2 layers separated keep top layer(oil layer)
6. Bottom layer( water layer) is extracted with DCM, let the layers separate completely, add the bottom layer(DCM layer) to the layer kept in the point 5, mix them and evaporate DCM.(Optional)
7. The mixture is steam distilled at 140-145C to get a transparent oil, at 100C oil starts to run out in the cooler at 130C turn on the steam and don't heat it more than 150C in that case you will get yellow oil.
8. Let separate completely the 2 layers of your distillation receiving flask, keep the top layer(oil layer)
9. Bottom layer( water layer) is extracted with DCM, let the layers separate completely, add the bottom layer(DCM layer) to the layer kept in the point 8, mix them, dry it with anhydrous Na2SO4 or MgSO4, filter it and evaporate DCM.(Optional)
10. 8,3L of amphetamine freebase obtained.

N-Formylamphetamine Hydrolysis by NaOH way
​

1. Put the 11L of N-Formylamphetamine in the reactor, add 13L previous cold 65% NaOH solution slow stirring with reflux during 2-3 hours at 110C.
2. Stop heating and cool it at RT
3. Keep the top layer(oil layer)
4. Bottom layer( water layer) is extracted with DCM, let the layers separate completely, add the bottom layer(DCM layer) to the layer kept in the point 3, mix them and evaporate DCM.(Optional)
5. The mixture is steam distilled at 140-145C to get a transparent oil, at 100C oil starts to run out in the cooler at 130C turn on the steam and don't heat it more than 150C in that case you will get yellow oil.
6. Let separate completely the 2 layers of your distillation receiving flask, keep the top layer(oil layer)
7. Bottom layer( water layer) is extracted with DCM, let the layers separate completely, add the bottom layer(DCM layer) to the layer kept in the point 6, mix them, dry it with anhydrous Na2SO4 or MgSO4, filter it and evaporate DCM.(Optional)
8. 8,5L of amphetamine freebase obtained.

​

btcboss2022Nice write up, can you tell me please how to prepair the 65% NaOH solution because I'm doing something wrong

 

[btcboss2022]

Nice write up, can you tell me please how to prepair the 65% NaOH solution because I'm doing something wrong

damakemiH2O(1L)+NaOH(650gr) technically is not in this way but will works anyway ;-)

 

[OrgUnikum]

H2O(1L)+NaOH(650gr) technically is not in this way but will works anyway ;-)

btcboss2022As you say its not so very correct. As what you prepare is regarded to be a 39% solution.
Such concentrations are always by weight say 40% NaOH means 1000 gram solution contain 400 g NaOH and 600g water. But in India a 100% solution is 1/1 by weight NaOH/water, well sometimes. International standard is as told though.

 

[btcboss2022]

As you say its not so very correct. As what you prepare is regarded to be a 39% solution.
Such concentrations are always by weight say 40% NaOH means 1000 gram solution contain 400 g NaOH and 600g water. But in India a 100% solution is 1/1 by weight NaOH/water, well sometimes. International standard is as told though.

OrgUnikumI know I know is exactly what I clarified and I only trying to make it simple because it will works anyway.

 

[damakemi]

H2O(1L)+NaOH(650gr) technically is not in this way but will works anyway ;-)

btcboss2022Thnx for answering, it's looks a whole lot different now. Did you only wash the p2p?

 

[btcboss2022]

Thnx for answering, it's looks a whole lot different now. Did you only wash the p2p?

damakemiYes bicarbonate solution.

 

[damakemi]

Yes bicarbonate solution.

btcboss202220% ?

 

[btcboss2022]

20% ?

damakemiI always dissolve 1.5kg in around 45L

 

[door]

The last result turn it in to crystal ?