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Here are the exactly details how I did, I must did it in these amounts because I didn't had enough sodium borohydride( new order arriving ;-)) and I used a big glass reactor so don't pay so much attention to the amounts the original synth posted here has the correct amounts of products, focus on the process only.
Synthesis:
1. Solution IPA/H2O 2:1 (10,4L) was added to the reactor and stir at room temp.
2. NaBH4 (500gr) was added at once while stirring.
3. P2NP (287gr) was added in small portions, so that the temperature of the mixture did not exceed 60 *С.
4. CuCl2 (30 g) in water (57,50 ml) was added at once the temperature of the mixture did not exceed 80 *С.
5. Thereafter, reaction was then held at 80 °C for 30 minutes using external heating.
6. The mixture is filtered with Buchner funnel to clean it from the solid waste of the CuCl2
7. 25% water solution of NaOH (2,3 liters) was added to reaction mixture stir 5 min and once stirring stopped leave separate phases 1 hour.
8. The aqueous phase was thereafter extracted with 2,3 liters of IPA.
9. The first layer separated is mixed with the IPA extraction and the mixture dried with anhydrous sodium sulfate, filtered with Buchner funnel.
10. IPA was evaporated on vacuum to an oil.
11. Water is added to the oil to make steam distillation.
12. The distilled mixture is extracted twice with DCM(around 250ml of DCM for each 2 liters of mixture)
13. Extraction is evaporated on vacuum in rotavap until gets off all the DCM.
14. 254gr of Amphetamine freebase are obtained(transparent oil with PH 13)
15. The cooled freebase is mixed with cold methanol(533ml).
16. 34,5 ml of cooled pure sulfuric acid was added slow dropwise while strong stirring until PH 6 during this process an increasingly dense paste is formed.
17. 790gr of amphetamine "pasta" are obtained.
18. The mixture was put in the freezer for 12 hours.
19. After this 12 hours you can choose if filter it and dry it to obtain the amphetamine sulfate(wash it with acetone with this clean and pure result won't change anything), or directly keep it as "pasta" form in freezer.
20. To consume the product from the "pasta" form take and small portion of it and spread it for example on a sheet of paper or on a hot plate until it dries.
Synthesis:
1. Solution IPA/H2O 2:1 (10,4L) was added to the reactor and stir at room temp.
2. NaBH4 (500gr) was added at once while stirring.
3. P2NP (287gr) was added in small portions, so that the temperature of the mixture did not exceed 60 *С.
4. CuCl2 (30 g) in water (57,50 ml) was added at once the temperature of the mixture did not exceed 80 *С.
5. Thereafter, reaction was then held at 80 °C for 30 minutes using external heating.
6. The mixture is filtered with Buchner funnel to clean it from the solid waste of the CuCl2
7. 25% water solution of NaOH (2,3 liters) was added to reaction mixture stir 5 min and once stirring stopped leave separate phases 1 hour.
8. The aqueous phase was thereafter extracted with 2,3 liters of IPA.
9. The first layer separated is mixed with the IPA extraction and the mixture dried with anhydrous sodium sulfate, filtered with Buchner funnel.
10. IPA was evaporated on vacuum to an oil.
11. Water is added to the oil to make steam distillation.
12. The distilled mixture is extracted twice with DCM(around 250ml of DCM for each 2 liters of mixture)
13. Extraction is evaporated on vacuum in rotavap until gets off all the DCM.
14. 254gr of Amphetamine freebase are obtained(transparent oil with PH 13)
15. The cooled freebase is mixed with cold methanol(533ml).
16. 34,5 ml of cooled pure sulfuric acid was added slow dropwise while strong stirring until PH 6 during this process an increasingly dense paste is formed.
17. 790gr of amphetamine "pasta" are obtained.
18. The mixture was put in the freezer for 12 hours.
19. After this 12 hours you can choose if filter it and dry it to obtain the amphetamine sulfate(wash it with acetone with this clean and pure result won't change anything), or directly keep it as "pasta" form in freezer.
20. To consume the product from the "pasta" form take and small portion of it and spread it for example on a sheet of paper or on a hot plate until it dries.
After evaporating ipa in a rotary evaporator, i always get an oil that does not separate from the water when water is added for the subsequent steam distillation and therefore does not float on top, it is a homogeneous solution, if i then steam distil fiese, i also get a homogeneous cloudy solution in the receiving flask. What could be the reason for this? does anyone know what I am doing wrong? Please help!