反应详情

To a solution of 5-bromo-2,3-difluorophenol (19 g, 90 mmol) in acetone (180 mL), K2CO3 (18 g, 0.13 mol) and iodomethane (25.8 g, 0.18 mol) were added. The resulting mixture was refluxed for 4 h. Upon completion, the mixture was cooled to room temperature and filtered, and the filtrate was evaporated to give the crude product, which was further purified by column chromatography on silica gel (eluting with petroleum ether/ethyl acetate=80/1˜40/1) to give a light yellow liquid 5-bromo-1,2-difluoro-3-methoxybenzene (19 g). 1H NMR (CDCl3): δ 7.00-6.88 (m, 2H), 3.89 (s, 3H).

1. temperatureThe resulting mixture was refluxed for 4 h
2. filtrationfiltered
3. customthe filtrate was evaporated
4. customto give the crude product, which
5. customwas further purified by column chromatography on silica gel (eluting with petroleum ether/ethyl acetate=80/1˜40/1)