反应详情

温度

-78 °C

To a solution of 1-(p-tolyl)ethanone (609 mg, 4.31 mmol) in THF (10 mL) was cooled to −78° C. and to this solution was added lithium bis(trimethylsilyl)amide (4.31 mL, 4.31 mmol). The resulting mixture was stirred at −78° C. for 20 min and then Intermediate 8C (620 mg, 1.437 mmol) in THF (3 mL) was added dropwise. The resulting mixture was stirred at −78° C. for 1.5 h and then at 0° C. for 1.5 h. The reaction was quenched with NH4Cl and concentrated. The crude product was purified by silica gel chromatography (80 g silica gel, eluted with EtOAc in hexanes) to afford Intermediate 8D (482 mg, 59%) as the slower eluting diastereomer on silica gel column. LCMS Anal. Calc'd for C27H33F6NO3S 565.21, found [M+H] 566.0.

1. stirringThe resulting mixture was stirred at −78° C. for 1.5 h
2. waitat 0° C. for 1.5 h
3. customThe reaction was quenched with NH4Cl
4. concentrationconcentrated
5. customThe crude product was purified by silica gel chromatography (80 g silica gel, eluted with EtOAc in hexanes)