Need help convert bmk 5449-12-7 to free base A-oil
- Thread starter Saul
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hello my friend I have some questions off this pdf
what is the differ ens between commercial p2p and impure p2p ?
what is 5 eq mean ? is it if you have 100ml that you use 500ml off it ? and how do you do this if the substance is in powder form ?
and last what they mean with excess formic acid ?
what is the differ ens between commercial p2p and impure p2p ?
what is 5 eq mean ? is it if you have 100ml that you use 500ml off it ? and how do you do this if the substance is in powder form ?
and last what they mean with excess formic acid ?
An impure molecule, as the name suggests, is a molecule mixed with, for example, traces of solvent or another molecule. (Water, acid, etc) Hence the importance of separating, cleaning, distilling and drying the p2p.
This will become more technical.
We're talking about "mole" ratios.
In this case, you want to react the p2p with the ammonium carbonate-formic acid mixture.
The most interesting method for you, since you don't know the purity of your final p2p production, is ammonium carbonate (5eq) and formic acid in excess.
Let's make it more concrete for you. Let's do some maths:
Let's imagine 100mL of P2P (relatively pure as it is cleaned, distilled and dried) which has a mass of 101g. (The density of P2P is 1.01g/mL)
The number of moles is obtained by dividing the mass by the molar mass. The molar mass of P2P is 134.175g/mol. (This means that if you have +-134g of P2P, you have one mole.)
So in the case of 101g of P2P (100mL), if we divide 101 by 134.18 we get 0.75 mol of P2P.
According to the PDF document put in the conversation earlier. The ratio of the reaction is 1:5:Excess (1 is P2P, 5 is ammonium carbonate and excess formic acid)
Let's apply this to our 0.75 mol P2P.
We must have 5 x 0.75 moles of ammonium carbonate or 3.75 moles. Knowing that the molar mass of ammonium carbonate is 96.085g/mol, you need 360g of ammonium carbonate.
The excess of formic acid means that you want to react the formic acid completely with the ammonium carbonate, but that in addition there must still be formic acid in the medium.
In the document it is stated that a slight excess is sufficient. We will use 8 moles of formic acid or 433g.
In summary:
1) Take a 2L round-bottomed flask and add 433g of formic acid. Add slowly and in small quantities the 360g of ammonium carbonate. Wait between additions until the effervescence of CO2 stops. If this is not respected, there is a risk of overflowing.
2) Added to the prepared solution the 100mL of P2P.
3) Connected in reflux under good agitation.
4) Maintain a temperature of 160-165°C for 24 hours. You can do it in several 6-hour sessions, for example.
N-Formylamphetamine is the product with a yield up to 78%. (A-Oil)
This procedure is based on the document and I have not tested it but it comes from the extensively detailed thesis so I think it must be correct.
My calculations are based on 85% formic acid which is the commercial standard.
From a personal point of view and as a chemist this seems more than correct and feasible.
If you want to work with 200mL, just double the mass of formic acid and ammonium carbonate and so on.
This will become more technical.
We're talking about "mole" ratios.
In this case, you want to react the p2p with the ammonium carbonate-formic acid mixture.
The most interesting method for you, since you don't know the purity of your final p2p production, is ammonium carbonate (5eq) and formic acid in excess.
Let's make it more concrete for you. Let's do some maths:
Let's imagine 100mL of P2P (relatively pure as it is cleaned, distilled and dried) which has a mass of 101g. (The density of P2P is 1.01g/mL)
The number of moles is obtained by dividing the mass by the molar mass. The molar mass of P2P is 134.175g/mol. (This means that if you have +-134g of P2P, you have one mole.)
So in the case of 101g of P2P (100mL), if we divide 101 by 134.18 we get 0.75 mol of P2P.
According to the PDF document put in the conversation earlier. The ratio of the reaction is 1:5:Excess (1 is P2P, 5 is ammonium carbonate and excess formic acid)
Let's apply this to our 0.75 mol P2P.
We must have 5 x 0.75 moles of ammonium carbonate or 3.75 moles. Knowing that the molar mass of ammonium carbonate is 96.085g/mol, you need 360g of ammonium carbonate.
The excess of formic acid means that you want to react the formic acid completely with the ammonium carbonate, but that in addition there must still be formic acid in the medium.
In the document it is stated that a slight excess is sufficient. We will use 8 moles of formic acid or 433g.
In summary:
1) Take a 2L round-bottomed flask and add 433g of formic acid. Add slowly and in small quantities the 360g of ammonium carbonate. Wait between additions until the effervescence of CO2 stops. If this is not respected, there is a risk of overflowing.
2) Added to the prepared solution the 100mL of P2P.
3) Connected in reflux under good agitation.
4) Maintain a temperature of 160-165°C for 24 hours. You can do it in several 6-hour sessions, for example.
N-Formylamphetamine is the product with a yield up to 78%. (A-Oil)
This procedure is based on the document and I have not tested it but it comes from the extensively detailed thesis so I think it must be correct.
My calculations are based on 85% formic acid which is the commercial standard.
From a personal point of view and as a chemist this seems more than correct and feasible.
If you want to work with 200mL, just double the mass of formic acid and ammonium carbonate and so on.
started the sequel today. I only used 100mg p2p
this video is after 4 hours cooking
this photo is after 4 hours of cooking
this photo is after 6 hours cooking and leth it cool down a wile
this video is after 4 hours cooking
http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/data/video/6/6292-c2bcacef613e32134eacf947334faa50.mp4
this photo is after 4 hours of cooking
http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/attachments/lmzswe2pfx-jpg.6291/?hash=ec8ecc91fdfa43e76b1a6d98e54266c7
this photo is after 6 hours cooking and leth it cool down a wile
http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/attachments/nnjalc8l6u-jpg.6290/?hash=ec8ecc91fdfa43e76b1a6d98e54266c7
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hello serialz
I have some questions
you saw my picture after 6 hours of cooking.
so 6 hours later I cooked again for 6 hours.
but the oil has turned very dark and less amount.
I think I had the best result after 4 hours off cooking.
I didn't measure the amount at the time but I think it was short with 100ml of verry light yellow collor.
any idea what goes wrong ?
"Amphetamine has been synthesised from l-phenyl-2-propanone (P2P) via
N-formylamphetamine using ammonium formate. l-Phenyl-2-propanone and
ammonium formate, (...) were combined and heated (160-180° C )
The contents of the distillation flask were then cooled and hydrolysed by
heating with concentrated hydrochloric acid for 3 hours. The reaction mixture was
washed with benzene-(Toluene should work too) (to remove unreacted ketone ), made alkaline, and steam distilled.
The distillate was extracted with benzene (Toluene should work too) and the product distilled to afford l-phenyl-2-
aminopropane (amphetamine)"
Absolutely respect the 4x6 hours of reflux. Then do what it says above.
As I have indicated to you, I have not personally used this route to synthesis.
So there are many factors that can make it not work.
Keep us informed ;-)
N-formylamphetamine using ammonium formate. l-Phenyl-2-propanone and
ammonium formate, (...) were combined and heated (160-180° C )
The contents of the distillation flask were then cooled and hydrolysed by
heating with concentrated hydrochloric acid for 3 hours. The reaction mixture was
washed with benzene-(Toluene should work too) (to remove unreacted ketone ), made alkaline, and steam distilled.
The distillate was extracted with benzene (Toluene should work too) and the product distilled to afford l-phenyl-2-
aminopropane (amphetamine)"
Absolutely respect the 4x6 hours of reflux. Then do what it says above.
As I have indicated to you, I have not personally used this route to synthesis.
So there are many factors that can make it not work.
Keep us informed ;-)
This is what you did for 24 hours (4x6h) and that led to your "A-Oil":
"Amphetamine has been synthesised from l-phenyl-2-propanone (P2P) via
N-formylamphetamine using ammonium formate. l-Phenyl-2-propanone and
ammonium formate, (...) were combined and heated (160-180° C )"
But your "A-Oil" must be treated with HCl as indicated here:
"The contents of the distillation flask were then cooled and hydrolysed by
heating with concentrated hydrochloric acid for 3 hours. The reaction mixture was
washed with benzene-(Toluene should work too) (to remove unreacted ketone ), made alkaline, and steam distilled.
The distillate was extracted with benzene (Toluene should work too) and the product distilled to afford l-phenyl-2-
aminopropane (amphetamine)"
All this is done in one glassware, your 24 hours of reflux and then the treatment of the "A-Oil" obtained after the 24 hours of reflux.
You can't isolate your A-Oil (you could but it would be complicated for you.) What I'm doing here is simplifying your life. I'm sorry you don't understand but unfortunately there is nothing I can do about it.
As mentioned above, I can't tell you if it doesn't work what the problem might be. It could be metal contamination from your stirrer that you dissolved when making the P2P. Another contaminant. A bad separation of the P2P that still had phosphoric or sulphuric acid. Etc etc etc
The list can be long. I can guide you as a chemist but not for you ;-)
So go to the end of your 24H of reflux, make the medium acid with HCl (pH2).
Then do the reflux as indicated for extraction etc. And you may get some amphetamine at the end.
But please don't be sarcastic with me.
You wanted to go that route with ammonium carbonate, not me ^^
Even though there were much simpler ways to synthesize it.
I've just been "trying" to guide you since the beginning.
"Amphetamine has been synthesised from l-phenyl-2-propanone (P2P) via
N-formylamphetamine using ammonium formate. l-Phenyl-2-propanone and
ammonium formate, (...) were combined and heated (160-180° C )"
But your "A-Oil" must be treated with HCl as indicated here:
"The contents of the distillation flask were then cooled and hydrolysed by
heating with concentrated hydrochloric acid for 3 hours. The reaction mixture was
washed with benzene-(Toluene should work too) (to remove unreacted ketone ), made alkaline, and steam distilled.
The distillate was extracted with benzene (Toluene should work too) and the product distilled to afford l-phenyl-2-
aminopropane (amphetamine)"
All this is done in one glassware, your 24 hours of reflux and then the treatment of the "A-Oil" obtained after the 24 hours of reflux.
You can't isolate your A-Oil (you could but it would be complicated for you.) What I'm doing here is simplifying your life. I'm sorry you don't understand but unfortunately there is nothing I can do about it.
As mentioned above, I can't tell you if it doesn't work what the problem might be. It could be metal contamination from your stirrer that you dissolved when making the P2P. Another contaminant. A bad separation of the P2P that still had phosphoric or sulphuric acid. Etc etc etc
The list can be long. I can guide you as a chemist but not for you ;-)
So go to the end of your 24H of reflux, make the medium acid with HCl (pH2).
Then do the reflux as indicated for extraction etc. And you may get some amphetamine at the end.
But please don't be sarcastic with me.
You wanted to go that route with ammonium carbonate, not me ^^
Even though there were much simpler ways to synthesize it.
I've just been "trying" to guide you since the beginning.