Hydrochloric Acid → Phenacylamine

Temperature

60 °C

2-Bromoacetophenone (18 g, 90 mmol) was dissolved in 900 ml of chloroform. Hexamethylenetetraamine (13.87 g, 99 mmol) was added thereto and the reaction mixture was stirred at 60° C. for 4 hours. After stirring, the reaction mixture was cooled down to room temperature, filtered, and the collected precipitate was suspended in 180 ml of ethanol. To the suspension thus obtained was added dropwise 90 ml of conc. HCl, and the reaction mixture was stirred at room temperature for 18 hours. Then, the reaction mixture was filtered to remove a white precipitate, the filtrate was concentrated under reduced pressure to obtain a yellow solid. This solid was recrystallized from a mixture of methanol and ethyl acetate (1:50, v/v) to obtain 13 g of 2-aminoacetophenone as a yellow solid.

1. stirringAfter stirring
2. temperaturethe reaction mixture was cooled down to room temperature
3. filtrationfiltered
4. customTo the suspension thus obtained
5. stirringthe reaction mixture was stirred at room temperature for 18 hours
6. filtrationThen, the reaction mixture was filtered
7. customto remove a white precipitate
8. concentrationthe filtrate was concentrated under reduced pressure
9. customto obtain a yellow solid
10. customThis solid was recrystallized from a mixture of methanol and ethyl acetate (1:50

ORD record

ord-d87fcbb348594ae197b7cdccac7b5e76

Source dataset

uspto-grants-1999_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05932742