反应详情

131 g of 4-(4-chloro-phenylsulfanyl)-6-ethyl-5-fluoropyrimidine, 103.8 g of N-bromosuccinimide and 7.98 g of azobisisobutyronitrile were dissolved in 850 ml of dichloroethane. The resulting mixture was refluxed for 2 hours, cooled to room temperature, and washed successively with 800 ml of water, 50 g of sodium metabisulfite in 950 ml of water and 500 ml of brine. The resulting solution was concentrated under a reduced pressure and crystallized at 5° C. in 391 ml of isopropanol to obtain the white compound, and the compound was washed with 50 ml of isopropanol at 5° C. to obtain the white title compound (150.7 g, yield: 89%).

1. temperatureThe resulting mixture was refluxed for 2 hours
2. washwashed successively with 800 ml of water, 50 g of sodium metabisulfite in 950 ml of water and 500 ml of brine
3. concentrationThe resulting solution was concentrated under a reduced pressure
4. customcrystallized at 5° C. in 391 ml of isopropanol
5. customto obtain the white compound
6. washthe compound was washed with 50 ml of isopropanol at 5° C.