反应详情

温度

0 °C

Dissolve under nitrogen atmosphere (2-fluoro-4-phenoxyphenyl)-methanol (1.41 g, 6.5 mmol) in anhydrous THF (60 mL). Cool to 0° C. in an ice bath. Add phosphorous tribromide (2.11 g, 7.8 mmol). Stir at cold for 1 h, then remove the ice bath and stir at ambient temperature for 16 h. Quench the reaction with saturated aqueous NaHCO3. Extract aqueous phase three times with EtOAc. Combine organic fractions, wash with brine, dry over Na2SO4 and concentrate in vacuo. Purify by chromatography on silica gel eluting with hexane/EtOAc (9:1). Evaporate the solvent to obtain the title compound (1.31 g, 72%).

1. customremove the ice bath
2. stirringstir at ambient temperature for 16 h
3. customQuench
4. customthe reaction with saturated aqueous NaHCO3
5. washCombine organic fractions, wash with brine
6. dry with materialdry over Na2SO4
7. concentrationconcentrate in vacuo
8. customPurify by chromatography on silica gel eluting with hexane/EtOAc (9:1)
9. customEvaporate the solvent