反应详情

To a solution of the compound prepared in Example 64 (2.41 g, 4.4 mmol) in acetonitrile (50 mL) and N,N-dimethylformamide (20 mL) at 0° C. was added N-chlorosuccinimide (0.62 g, 4.6 mmol). The reaction was warmed to room temperature, stirred under nitrogen overnight then heated between 50-70° C. for 2 h. The reaction was cooled to room temperature, concentrated under reduced pressure and the residue washed with aqueous sodium bicarbonate solution (1×50 mL). The solid residue was suspended in a mixture of ethyl acetate (100 mL) and dichloromethane (100 mL) and sonicated. The solids were collected by filtration to give the title compound (1.39 g) as an off-white solid.

1. temperaturethen heated between 50-70° C. for 2 h
2. temperatureThe reaction was cooled to room temperature
3. concentrationconcentrated under reduced pressure
4. washthe residue washed with aqueous sodium bicarbonate solution (1×50 mL)
5. additionThe solid residue was suspended in a mixture of ethyl acetate (100 mL) and dichloromethane (100 mL)
6. customsonicated
7. filtrationThe solids were collected by filtration