反应详情

温度

0 °C

To a solution of the compound of Example 1 (5.0 g, 6.9 mmol) and methyl sulfide (4.1 mL) in acetonitrile (35 mL) at 0° C. was added benzoyl peroxide (6.7 g) in four portions over 20 minutes, and the mixture was stirred at 0° C. for 1 hour and then at room temperature for 1 hour. The reaction was diluted with ethyl acetate and washed with 10% Na2CO3 and brine. The organic was dried over MgSO4, filtered and evaporated. The residue was chromatographed on silica gel eluting with a gradient of 33-100% ethyl acetate in chloroform to give the title compound (4.56 g, 84% yield).

1. waitat room temperature for 1 hour
2. washwashed with 10% Na2CO3 and brine
3. dry with materialThe organic was dried over MgSO4
4. filtrationfiltered
5. customevaporated
6. customThe residue was chromatographed on silica gel eluting with a gradient of 33-100% ethyl acetate in chloroform