反应详情

(6-Fluoro-benzo[1,3]dioxol-5-yl)-methanol (650 mg, 3.8 mmol) was added to SOCl2 (20 mL) in portions at 0° C. The mixture was warmed to room temperature for 1 h and then heated at reflux for 1 h. The excess SOCl2 was evaporated under reduced pressure to give the crude product, which was basified with sat. NaHCO3 solution to pH ˜7. The aqueous phase was extracted with EtOAc (50 mL×3). The combined organic layers were dried over Na2SO4 and evaporated under reduced pressure to give 5-chloromethyl-6-fluoro-benzo[1,3]dioxole (640 mg, 90%), which was directly used in the next step.

1. temperatureheated
2. temperatureat reflux for 1 h
3. customThe excess SOCl2 was evaporated under reduced pressure
4. customto give the crude product, which
5. extractionThe aqueous phase was extracted with EtOAc (50 mL×3)
6. dry with materialThe combined organic layers were dried over Na2SO4
7. customevaporated under reduced pressure