Azobisisobutyronitrile → HCID 25184799、化合物
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][C:9]2[C:14]([F:15])=[C:13]([CH2:16][CH3:17])[N:12]=[CH:11][N:10]=2)=[CH:4][CH:3]=1.[Br:18]N1C(=O)CCC1=O.N(C(C)(C)C#N)=NC(C)(C)C#N>ClC(Cl)C>[Br:18][CH:16]([C:13]1[C:14]([F:15])=[C:9]([S:8][C:5]2[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][CH:6]=2)[N:10]=[CH:11][N:12]=1)[CH3:17]参加物
5
実験手順
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%).