反应详情

温度

-2.5 °C

At −5-0° C., ethoxybenzene (20.5 g) and AlCl3 (22.3 g) were added into a solution of 5-bromo-2-chlorobenzoyl chloride (from step 2) in dry DCM (200 mL). Then the mixture was stirred at −5-0° C. for 1 h. The mixture was poured into ice-H2O (200 mL) and extracted with DCM. The organic phase was washed with 1M HCl, H2O, IM NaOH and brine. And the organic phase was concentrated, and the crude was purified by silica-gel column chromatography (PE/EA=80/1-40/1), to obtain 30 g of (5-bromo-2-chloro phenyl)(4-ethoxyphenyl)methanone.

1. extractionextracted with DCM
2. washThe organic phase was washed with 1M HCl, H2O, IM NaOH and brine
3. concentrationAnd the organic phase was concentrated
4. customthe crude was purified by silica-gel column chromatography (PE/EA=80/1-40/1)