反应详情

A mixture of 2-bromo-3′,4′-dichloroacetophenone (78.0 g), sodium formate (68.0 g) and methanol (300 mL) was heated under reflux and stirred for 16 h. The reaction mixture was concentrated and poured into water (1 L). The precipitated solid was collected by filtration, washed with water and then with isopropyl ether, air-dried, and further dried under reduced pressure at 40° C. to give the title compound as crystals (25.0 g, 42%). Recrystallization from ethyl acetate-hexane gave pale-yellow prism crystals. melting point: 115-118° C.

1. temperaturewas heated
2. temperatureunder reflux
3. concentrationThe reaction mixture was concentrated
4. additionpoured into water (1 L)
5. filtrationThe precipitated solid was collected by filtration
6. washwashed with water
7. dry with materialwith isopropyl ether, air-dried
8. customfurther dried under reduced pressure at 40° C.