反应详情

温度

-78 °C

To a solution of 76A (380 mg, 1.01 mmol) in THF (5 mL) at −78° C., was added NaHMDS (1.3 mL, 1.0M, 1.3 mmol), dropwise. The solution was stirred at −78° C. for 3 h. A solution of MeI (0.62 mL, 10 mmol) in 2 mL THF was added. The solution was stirred −78° C. for 3 h, and −40° C. for 1 h. The reaction was quenched with sat. NH4Cl and extracted with EtOAc (3×20 mL). The organic layer washed with brine, dried (Na2SO4), and concentrated. Purification via flash chromatography (0-30% EtOAc in hexanes) gives 76B (70 mg, 18%). MS (ESI) m/z 388.3 (M+H)+.

1. stirringThe solution was stirred −78° C. for 3 h
2. wait−40° C. for 1 h
3. customThe reaction was quenched with sat. NH4Cl
4. extractionextracted with EtOAc (3×20 mL)
5. washThe organic layer washed with brine
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated
8. customPurification via flash chromatography (0-30% EtOAc in hexanes)