反应详情

温度

0 °C

To a solution of 60 (15.12 g, 64.79 mmol) and THF (50 mL) cooled to 0° C. was added dropwise (4-chloro-3-fluorophenyl)magnesium bromide (226.8 mL, 113.4 mmol) and the solution was stirred at 0° C. for 2 h. Saturated NH4Cl was added and the reaction was extracted with DCM. The organic layer was separated, dried, filtered and concentrated. The crude product was purified by passage through a SiO2 plug eluting with 5% EtOAc/hexane to afford 18.36 g (93.6%) of 2-(tert-butyldimethylsilyloxy)-1-(4-chloro-3-fluorophenyl)ethanone (62).

1. extractionthe reaction was extracted with DCM
2. customThe organic layer was separated
3. customdried
4. filtrationfiltered
5. concentrationconcentrated
6. customThe crude product was purified by passage through a SiO2 plug
7. washeluting with 5% EtOAc/hexane