Good method, congratulations. Why didn't you choose the method of obtaining amphetamine through 1-phenyl-2-nitropene > 1-phenyl-2-nitropropane > ZINC + hydrochloric acid?
The volumes scale more and the temperature is more stable.
The yield of the final product is much higher
The consumption of NaBH4 during the formation of propane at 0-5 degrees is much less, and the yield of the final propane is higher.
Do you think it's enough to get the amphetamine base in isopropanol without additional fractional distillation?
Do you think that the final product does not contain borates?
The volumes scale more and the temperature is more stable.
The yield of the final product is much higher
The consumption of NaBH4 during the formation of propane at 0-5 degrees is much less, and the yield of the final propane is higher.
Do you think it's enough to get the amphetamine base in isopropanol without additional fractional distillation?
Do you think that the final product does not contain borates?
is this the way it is?
5000 ml three-neck, flat-bottomed flasks. placed in an ice bath and placed on a magnetic stirrer. We install a reflux condenser cooled with running water, a dropper with a pressure compensator and a thermometer.
In the flask we put 70 gr. NaBH4 dissolved in a mixture of 300 ml water and 700 ml IPA.
We drop a solution of 108 gr. P2NP in 200 ml. IPA through an addition funnel, at such a rate that the temperature of the reaction mixture does not rise above 5 degrees.
After adding all the propene in the flask, a white slurry with insoluble borates formed in the flask, cool the mixture to 0 degrees and slowly add 300 mL. chilled 85% acetic acid, keeping the temperature in the flask no higher than 3 degrees. When all the acetic acid has been added, the borates should dissolve and the solution should take on a yellowish beige hue.
We fall asleep in a flask with one portion of 270 gr. zinc dust and add 800 ml through the funnel. 38% hydrochloric acid in the amount of about 50-60 ml. in a minute. Then leave the mixture to stir for 2 hours.
The precipitate is additionally filtered by washing it on the filter with 2-3 portions of IPA, 20-30 ml each. the filtrate must be completely transparent. If there are any foreign inclusions, solid particles, filter again.
Add cooled 50% NaOH aqueous solution to the filtrate until a layer of yellowish oil comes to the surface, which will be separated, and the aqueous layer is washed 3-4 times with 100 ml. IPS. Combine the separated oil and alcohol extracts, add 50 gr. finely ground sodium sulfate, cool the mixture below 0 degrees and hold at this temperature for 2-3 hours. Then the mixture is filtered, the precipitate is washed on the filter 1-2 times with 50 ml. anhydrous IPS.
Add 200 ml to the filtrate. anhydrous acetone, put the mixture on a stirrer and add 96% sulfuric acid dropwise until the acidity of the mixture reaches 5.5 - 6. Already during the addition, a precipitate forms, it is necessary to stir the mixture throughout the volume. If mixing is difficult, a little anhydrous acetone can be added.
After reaching the required acidity, the precipitate is filtered, washed on the filter with a small amount of acetone until completely white and dried in air (or batteries) to constant weight. We get 100 + -10 gr. d,l-amphetamine sulfate.
If necessary, solvents can be distilled from the filtrate, the precipitate can be dissolved in 30-50 ml. anhydrous acetone and get another 5-15 g of the substance. However, these residues are quite dirty and will take a long time to wash through the filter, and recrystallization from an ethanol-water system may be necessary to achieve the same purity as the original product.
5000 ml three-neck, flat-bottomed flasks. placed in an ice bath and placed on a magnetic stirrer. We install a reflux condenser cooled with running water, a dropper with a pressure compensator and a thermometer.
In the flask we put 70 gr. NaBH4 dissolved in a mixture of 300 ml water and 700 ml IPA.
We drop a solution of 108 gr. P2NP in 200 ml. IPA through an addition funnel, at such a rate that the temperature of the reaction mixture does not rise above 5 degrees.
After adding all the propene in the flask, a white slurry with insoluble borates formed in the flask, cool the mixture to 0 degrees and slowly add 300 mL. chilled 85% acetic acid, keeping the temperature in the flask no higher than 3 degrees. When all the acetic acid has been added, the borates should dissolve and the solution should take on a yellowish beige hue.
We fall asleep in a flask with one portion of 270 gr. zinc dust and add 800 ml through the funnel. 38% hydrochloric acid in the amount of about 50-60 ml. in a minute. Then leave the mixture to stir for 2 hours.
The precipitate is additionally filtered by washing it on the filter with 2-3 portions of IPA, 20-30 ml each. the filtrate must be completely transparent. If there are any foreign inclusions, solid particles, filter again.
Add cooled 50% NaOH aqueous solution to the filtrate until a layer of yellowish oil comes to the surface, which will be separated, and the aqueous layer is washed 3-4 times with 100 ml. IPS. Combine the separated oil and alcohol extracts, add 50 gr. finely ground sodium sulfate, cool the mixture below 0 degrees and hold at this temperature for 2-3 hours. Then the mixture is filtered, the precipitate is washed on the filter 1-2 times with 50 ml. anhydrous IPS.
Add 200 ml to the filtrate. anhydrous acetone, put the mixture on a stirrer and add 96% sulfuric acid dropwise until the acidity of the mixture reaches 5.5 - 6. Already during the addition, a precipitate forms, it is necessary to stir the mixture throughout the volume. If mixing is difficult, a little anhydrous acetone can be added.
After reaching the required acidity, the precipitate is filtered, washed on the filter with a small amount of acetone until completely white and dried in air (or batteries) to constant weight. We get 100 + -10 gr. d,l-amphetamine sulfate.
If necessary, solvents can be distilled from the filtrate, the precipitate can be dissolved in 30-50 ml. anhydrous acetone and get another 5-15 g of the substance. However, these residues are quite dirty and will take a long time to wash through the filter, and recrystallization from an ethanol-water system may be necessary to achieve the same purity as the original product.
Attachments
Yes, +- this method. The main task in the formation of propane with a large yield.
Also use an overhead stirrer to stir the zinc.
Also use an overhead stirrer to stir the zinc.
