反应详情

温度

-20 °C

A solution of Example 22A (325 mg, 1 mmol) and iodomethane (0.12 ml, 2.0 mmol) in THF (5 mL) was treated with NaN(TMS)2 in THF (1.0 M, 2 mL, 2.0 mmol) at −70° C. under nitrogen. The temperature of the cooling bath was slowly raised to −20° C. within 1 h and the mixture was stirred at the same temperature for additional 2 h. After quenching with water, the mixture was partitioned between water and EtOAc. The organic phase was washed with water and concentrated. The residue was purified on flash column chromatograph to give Example 22B. (250 mg, 77% yield). MS (DCI/NH3) m/z 340 (M+H)+.

1. customAfter quenching with water
2. customthe mixture was partitioned between water and EtOAc
3. washThe organic phase was washed with water
4. concentrationconcentrated
5. customThe residue was purified on flash column chromatograph
6. customto give Example 22B