反应详情

To SOCl2 (20 mL) was added (7-fluoro-benzo[1,3]dioxol-5-yl)-methanol (0.80 g, 4.7 mmol) in portions at 0° C. The mixture was warmed to room temperature over 1 h and then was heated at reflux for 1 h. The excess SOCl2 was evaporated under reduced pressure to give the crude product, which was basified with saturated aqueous NaHCO3 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 6-chloromethyl-4-fluoro-benzo[1,3]dioxole (0.80 g, 92%), which was directly used in the next step.

1. temperaturewas heated
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