反应详情

温度

50 °C

A solution of bromine (0.31 g, 1.95 mmol) in 1.0 ml glacial acetic acid was added to a stirred solution of 5-chlorobenzo[b]thiophene (0.300 g, 1.77 mmol)in glacial acetic acid (1.0 ml) under nitrogen atmosphere. The reaction was heated to 50° C. for 4 hours, the volatiles removed under reduced pressure, the residue diluted in methylene chloride, washed with aq. sodium bicarbonate and with brine and dried over sodium sulfate. Evaporation gave 0.335 g (76%) of a tan solid. mp 85°-86° C., FDMS m/e=249 (M+2).

1. customthe volatiles removed under reduced pressure
2. additionthe residue diluted in methylene chloride
3. washwashed with aq. sodium bicarbonate and with brine
4. dry with materialdried over sodium sulfate
5. customEvaporation