反应详情

Hexamethylenetetramine (1.42 g, 10.1 mmol) was added dropwise over 30 min to a solution of 2-bromo-4-fluoroacetophenone (2.0 g, 9.2 mmol) in dry CHCl3 (40 mL) at 0° C. The reaction mixture was allowed to warm up to room temperature and stirred for 16 h. After completion of the reaction the solid precipitate formed was collected by filtration and washed with CHCl3. The solid obtained was suspended in EtOH (40 mL) and conc. HCl (4 mL) was added. The mixture was heated to 80° C. for 3 h, cooled to room temperature, and the solid formed was filtered off. The clear filtrate was concentrated to afford 2-amino-1-(4-fluorophenyl)ethanone hydrochloride (1.5 g, crude) as yellow solid. MS (ESI) m/z: Calculated for C8H8FNO: 153.06. found: 153.9 (M+H)+

1. customAfter completion of the reaction the solid precipitate
2. customformed
3. filtrationwas collected by filtration
4. washwashed with CHCl3
5. customThe solid obtained
6. temperatureThe mixture was heated to 80° C. for 3 h
7. temperaturecooled to room temperature
8. customthe solid formed
9. filtrationwas filtered off
10. concentrationThe clear filtrate was concentrated