反应详情

温度

55 °C

2-Bromo-1-(3-chlorophenyl)ethanone (2.0 g, 8.57 mmol) was added to a solution of hexamethylenetetramine (1.201 g, 8.57 mmol) in CHCl3 (60 mL), and the resulting mixture was heated at 55° C. for 1 hour. The mixture was cooled to room temperature, and the white precipitate was collected by filtration, washed with CHCl3, and dried in vacuo to afford 3.1 g. This white solid was suspended in a mixture of ethanol (50 mL) and hydrochloric acid (0.25 mL, 8.30 mmol) and heated at 105° C. for 1.5 hours. The mixture was cooled to 0° C., filtered and washed by ethanol (30 mL). The organic phase was concentrated to afford an HCl salt of the title compound (1.74 g) as a pale yellow solid. LC-MS (ES) m/z=170 [M+H]+.

1. temperatureThe mixture was cooled to room temperature
2. filtrationthe white precipitate was collected by filtration
3. washwashed with CHCl3
4. customdried in vacuo
5. customto afford 3.1 g
6. temperatureheated at 105° C. for 1.5 hours
7. temperatureThe mixture was cooled to 0° C.
8. filtrationfiltered
9. washwashed by ethanol (30 mL)
10. concentrationThe organic phase was concentrated