反应详情

温度

0 °C

To a solution of compound 53d (300 mg, 0.78 mmol) in DMF (3 mL) was added NaH (60% in mineral oil, 68.9 mg, 1.72 mmol) at 0° C. The mixture was stirred at 0° C. for 30 min, then CH3I (0.053 mL, 0.86 mmol) was added and stirring continued at 0° C. for another 1 h. The resulting mixture was diluted with EtOAc and water. The organic layer was washed with brine and concentrated. The residue was recrystallized from heptane, filtered and dried the solid to give compound 53f (265 mg) as a light yellow solid. MS m/z (M+H+) 284.1.

1. stirringstirring
2. waitcontinued at 0° C. for another 1 h
3. washThe organic layer was washed with brine
4. concentrationconcentrated
5. customThe residue was recrystallized from heptane
6. filtrationfiltered
7. customdried the solid