反应详情

A solution of (3,4-dichloro-phenyl)-acetic acid (10.0 g, 0.048 mol) in ethanol (50 mL) was treated with a catalytic amount of sulfuric acid. The reaction mixture was refluxed for 7 h. The reaction was concentrated in vacuo, diluted with diethyl ether, and poured into water. The ether layer was washed with a saturated aqueous sodium bicarbonate solution and water. The organics were then dried over sodium sulfate, filtered, and concentrated in vacuo. Vacuum distillation (bath temperature: 175° C.; head temperature: 125° C.) afforded (3,4-dichloro-phenyl)-acetic acid ethyl ester (9.38 g, 82.5%) as a clear oil: EI-HRMS m/e calcd for C10H10Cl2O2 (M+) 232.0058, found 232.0066.

1. temperatureThe reaction mixture was refluxed for 7 h
2. concentrationThe reaction was concentrated in vacuo
3. additiondiluted with diethyl ether
4. additionpoured into water
5. washThe ether layer was washed with a saturated aqueous sodium bicarbonate solution and water
6. dry with materialThe organics were then dried over sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. distillationVacuum distillation (bath temperature: 175° C.; head temperature: 125° C.)