反应详情

温度

0 °C

Potassium tert.-butoxide (1.12 g, 10.0 mmol) was added to a solution of 1-(3,4,5-trifluoro-phenyl)-ethanone (1.74 g, 10.0 mmol) and diethyl oxalate (1.49 mL, 11.0 mmol) in diethyl ether (20 mL) cooled to 0° C. The heterogenous mixture was stirred for 15 min at 0° C. followed by 15 h at 20° C. The mixture was partitioned between 3 N hydrochloric acid (20 mL) and diethyl ether (50 mL). The organic layer was washed with brine (20 mL), dried over sodium sulfate and evaporated under reduced pressure and the residual oil was crystallized from diethyl ether/heptane to give the title compound as a white solid.

1. waitfollowed by 15 h at 20° C
2. customThe mixture was partitioned between 3 N hydrochloric acid (20 mL) and diethyl ether (50 mL)
3. washThe organic layer was washed with brine (20 mL)
4. dry with materialdried over sodium sulfate
5. customevaporated under reduced pressure
6. customthe residual oil was crystallized from diethyl ether/heptane