反应详情

Bromine (1.2 mL, 23.0 mmol) in 10 mL of glacial acetic acid was added drop-wise to a solution of 1-(4-bromo-2-fluoro-phenyl)-ethanone (5.0 g, 23.0 mmol), prepared in the previous step, in 150 mL of dry methylene chloride at 0° C. After the addition, the reaction was allowed to warm to room temperature. TLC (5% ethyl acetate:hexane) indicated the starting material was consumed. The reaction was diluted with methylene chloride and washed with 5% sodium thiosulfate and brine. The organic layer was dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure to give 2-bromo-1-(4-bromo-2-fluoro-phenyl)-ethanone (6.6 g, 97%) as a light green oil. This compound was used without further purification. MS (ES) m/z 297 [M+H]+.

1. additionAfter the addition
2. customwas consumed
3. additionThe reaction was diluted with methylene chloride
4. washwashed with 5% sodium thiosulfate and brine
5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure