反应详情

To a solution of 4-bromo-3-chlorophenol (10.0 g), 3-ethoxypropanol (6.0 g) and triphenylphosphine (15.2 g) in tetrahydrofuran (50 ml) was added dropwise under nitrogen atmosphere at 0° C. diethylazodicarbonate (40% toluene solution, 25.2 g) for 15 minutes, and the mixture was stirred at room temperature for 2 hours and concentrated under reduced pressure. To the residue was added diethylether, and insoluble materials were filtered off. The filtrate was washed with saturated brine and dried with magnesium sulfate. Under reduced pressure, the solvent was evaporated, and the residue was purified with silica gel column chromatography (ethyl acetate/hexane 1:5) and distilled under reduced pressure (1.5 mmHg, 190° C.) to give colorless oil of 4-bromo-3-chloro-(3-ethoxypropoxy)benzene (11.2 g).

1. concentrationconcentrated under reduced pressure
2. additionTo the residue was added diethylether, and insoluble materials
3. filtrationwere filtered off
4. washThe filtrate was washed with saturated brine
5. dry with materialdried with magnesium sulfate
6. customUnder reduced pressure, the solvent was evaporated
7. customthe residue was purified with silica gel column chromatography (ethyl acetate/hexane 1:5)
8. distillationdistilled under reduced pressure (1.5 mmHg, 190° C.)