反应详情

Thionyl chloride (9.5 mL) was added dropwise to a solution of 4-chloro-2-(trifluoromethyl)phenylacetic acid (CAS #601513-31-9, 10.5 g) in methanol (50 mL) under ice-cooling. Then, the reaction solution was heated under reflux for three hours. The reaction solution was concentrated under reduced pressure. A saturated sodium bicarbonate solution and ethyl acetate were added to the resulting residue, and the organic layer was separated. The resulting organic layer was sequentially washed with a saturated sodium bicarbonate solution and brine, dried over anhydrous magnesium sulfate and then concentrated under reduced pressure to obtain 10.96 g of the title compound. 1H-NMR (CDCl3) δ (ppm): 3.71 (s, 3H), 3.80 (s, 2H), 7.35 (d, J=8.4 Hz, 1H), 7.50 (dd, J=8.4, 2.0 Hz, 1H), 7.65 (d, J=2.0 Hz, 1H).

1. temperaturecooling
2. temperatureThen, the reaction solution was heated
3. temperatureunder reflux for three hours
4. concentrationThe reaction solution was concentrated under reduced pressure
5. additionA saturated sodium bicarbonate solution and ethyl acetate were added to the resulting residue
6. customthe organic layer was separated
7. washThe resulting organic layer was sequentially washed with a saturated sodium bicarbonate solution and brine
8. dry with materialdried over anhydrous magnesium sulfate
9. concentrationconcentrated under reduced pressure