反应详情

To a solution of 2-(2-chloro-5-methoxy-4-nitrophenyl)ethanol (0.85 g, 3.67 mmol) in DCM (20 mL), triphenylphosphine (1.54 g, 5.9 mmol) and carbon tetrabromide (1.46 g, 4.4 mmol) were added. The reaction mixture was maintained for 7 hours at room temperature then partitioned between water (50 mL) and EtOAc (80 mL). The separated aqueous phase was extracted with EtOAc (80 mL), then the combined organic extracts were dried (Na2SO4) and concentrated under reduced pressure. The product was purified by column chromatography on neutral silica gel using 5-15% EtOAc in hexane to give the title compound (0.9 g, 83%) as a solid.

1. customthen partitioned between water (50 mL) and EtOAc (80 mL)
2. extractionThe separated aqueous phase was extracted with EtOAc (80 mL)
3. dry with materialthe combined organic extracts were dried (Na2SO4)
4. concentrationconcentrated under reduced pressure
5. customThe product was purified by column chromatography on neutral silica gel using 5-15% EtOAc in hexane