反应详情

温度

0 °C

To a solution of Intermediate 237.1 (30 mg, 0.04 mmol) in THF (1 mL) at 0° C. was added NaH (3.16 mg, 0.08 mmol), stirred at 0° C. for 30 min, then MeI was added and the reaction mixture was warmed up to rt over 1 h. The reaction mixture was then partitioned between EtOAc and sat. NH4Cl, the organic layer was dried (Na2SO4), filtered and concentrated. The crude product was purified by flash chromatography (0 to 100% EtOAc/hexanes, gradient) to afford 20 mg (62%) of Intermediate 237.2.

1. temperaturethe reaction mixture was warmed up to rt over 1 h
2. customThe reaction mixture was then partitioned between EtOAc and sat. NH4Cl
3. dry with materialthe organic layer was dried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated
6. customThe crude product was purified by flash chromatography (0 to 100% EtOAc/hexanes, gradient)