反应详情

温度

0 °C

To a solution of the compound of Example 1 (1.0 g, 1.38 mmol) and diisobutyl sulfide (6.2 mL) in acetonitrile (10 mL) at 0° C. was added benzoyl peroxide (2.0 g) in three portions over 30 minutes, and the reaction was stirred at 0° C. for 1 hour. The reaction was diluted with ethyl acetate and washed with 10% Na2CO3 and brine. The organic phase was dried over MgSO4, filtered and evaporated. The residue was chromatographed on silica gel eluting with a gradient starting with 0-100% ethyl acetate/dichloromethane to provide the title product (0.890 g, 75% yield).

1. washwashed with 10% Na2CO3 and brine
2. dry with materialThe organic phase was dried over MgSO4
3. filtrationfiltered
4. customevaporated
5. customThe residue was chromatographed on silica gel eluting with a gradient