反应详情

温度

180 °C

To a mixture of AlCl3 (37.5 g, 282.48 mmol) and NaCl (11 g, 188.32 mmol) was added 1-(4-bromo-2-fluoro-phenyl)-3-chloro-propan-1-one (5 g, 18.83 mmol) at 130° C. The reaction temperature was slowly increased to 180° C. and kept for 1 hour. It was cooled, the mixture was poured into ice and extracted twice with ethyl acetate (2×100 ml). The combined ethyl acetate phases were dried over Na2SO4 and evaporated to get the crude product which was purified by column chromatography (silica gel, 5-10% ethyl acetate/hexane) to give 2.4 g (55%) of the title compound as brown solid. MS: 229.2 (MH+, 1Br).

1. temperatureIt was cooled
2. additionthe mixture was poured into ice
3. extractionextracted twice with ethyl acetate (2×100 ml)
4. dry with materialThe combined ethyl acetate phases were dried over Na2SO4
5. customevaporated
6. customto get the crude product which
7. customwas purified by column chromatography (silica gel, 5-10% ethyl acetate/hexane)