反应详情

To a solution of the compound of Example 111 (1.4 g, 1.74 mmol) and methyl sulfide (3.2 mL, 43.3 mmol) in acetonitrile (18 mL) at 0° C. was added benzoyl peroxide (1.7 g), and the mixture was warmed to room temperature and stirred for 30 minutes. The reaction was cooled to 0° C. and benzoyl peroxide (1.7 g) was added, and the mixture was warmed to room temperature and stirred for 30 minutes. Water was added and 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 starting with dichloromethane and ending with ethyl acetate to give the title compound (1.24 g, 83% yield).

1. temperatureThe reaction was cooled to 0° C.
2. temperaturethe mixture was warmed to room temperature
3. stirringstirred for 30 minutes
4. washwashed with 10% Na2CO3 and brine
5. dry with materialThe organic was dried over MgSO4
6. filtrationfiltered
7. customevaporated
8. customThe residue was chromatographed on silica gel eluting with a gradient