反应详情

温度

-45 °C

The product of Example 438A (0.80 g, 3.8 mmol), di-tert-butyl diethylphosphoramidite (1.07 mL, 3.8 mmol), and 1-H-tetrazole (0.63 g, 8.99 mmol) in THF (35 mL) were reacted at room temperature for 12 hours. The reaction was diluted with dichloromethane (35 mL) and cooled to −45° C., and treated with mCPBA (0.90 g, 4.0 mmol) for 0.5 hours then diluted with ethyl acetate (100 mL). The organics were washed with 10% Na2CO3 (2×), brine, dried over MgSO4, and concentrated. The residue was purified by chromatography on silica gel, eluting with a gradient of ethyl acetate in dichloromethane (0-25%) to give the title compound as a colorless oil (0.926 g, 62%).

1. washThe organics were washed with 10% Na2CO3 (2×), brine
2. dry with materialdried over MgSO4
3. concentrationconcentrated
4. customThe residue was purified by chromatography on silica gel
5. washeluting with a gradient of ethyl acetate in dichloromethane (0-25%)