反应详情

温度

0 °C

To a solution of compound 11d (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 the solid dried to give compound 12a (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. customthe solid dried