反应详情

温度

48 °C

To 400 ml of chloroform in a 3 liter flask equipped with a mechanical stirrer was added 50 g of 2-bromo-4'-phenylacetophenone and 26.4 g of hexamethylenetetramine. The solution was stirred at 48° C. for 4 hours, then cooled to 20° C., and the resulting solid collected and washed with a small amount of absolute ethanol. The solid was suspended in a solution of 270 ml of absolute ethanol and 134 ml of concentrated hydrochloric acid and stirred at 20° C. for 22 hours. This solid was collected washed with 100 ml of water and dried at 75° C. in vacuo, giving 54.9 g of the desired compound as a white solid, mp 260° C.

1. temperaturecooled to 20° C.
2. customthe resulting solid collected
3. washwashed with a small amount of absolute ethanol
4. stirringstirred at 20° C. for 22 hours
5. customThis solid was collected
6. washwashed with 100 ml of water
7. customdried at 75° C. in vacuo