反应详情

温度

15 °C

To a stirred solution of ethyl 2-(4-hydroxyphenyl)acetate (25 g, 138 mmol) in 375 ml of DCM, sulfuryl chloride (9.48 mL 118 mmol) was slowly added at 0° C. over a period of 30 min. Diethyl ether (19.6 mL) was slowly added reaction mixture at 0° C. and stirring was continued for 30 min at 0° C. The reaction mixture was slowly warmed to 15° C. for 1 h. After completion of reaction, the mixture was poured onto crushed ice and extracted with DCM (×2). The combined organic layers were washed with 10% NaHCO3 solution followed by water. The organic layer was dried over Na2SO4, filtered and evaporated under vacuum to give compound ethyl 2-(3-chloro-4-hydroxyphenyl)acetate (15 g) as a thick oil.

1. customreaction mixture at 0° C.
2. customAfter completion of reaction
3. additionthe mixture was poured
4. customonto crushed ice
5. extractionextracted with DCM (×2)
6. washThe combined organic layers were washed with 10% NaHCO3 solution
7. dry with materialThe organic layer was dried over Na2SO4
8. filtrationfiltered
9. customevaporated under vacuum