Carbon Tetrachloride → HCID 178505887、化合物
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:16]2[C:11](=[N:12][C:13]([O:17][C:18]3[CH:23]=[CH:22][C:21]([F:24])=[CH:20][C:19]=3[F:25])=[CH:14][N:15]=2)[NH:10][N:9]=1.C(Cl)(Cl)(Cl)[Cl:27]>>[Cl:27][C:14]1[N:15]=[C:16]2[C:8]([C:3]3[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=3[Cl:1])=[N:9][NH:10][C:11]2=[N:12][C:13]=1[O:17][C:18]1[CH:23]=[CH:22][C:21]([F:24])=[CH:20][C:19]=1[F:25]参加物
3
実験手順
A suspension of 3-(2-chlorophenyl)-6-(2,4-difluorophenoxy)-1H-pyrazolo[3,4-b]pyrazine (2.70 g, 7.5 mmol) in 500 mL carbon tetrachloride was bubbled with chlorine gas for 16 hours at room temperature while stirring. The reaction mixture was concentrated under reduced pressure, and the residue was purified by chromatography (methylene chloride/hexanes 2:3 to 1:0) to give 1.21 g of 5-Chloro-3-(2-chloro-phenyl)-6-(2,4-difluoro-phenoxy)-1H-pyrazolo[3,4-b]pyrazine. Mass spec. M+1=394.
後処理
- customwas bubbled with chlorine gas for 16 hours at room temperature
- concentrationThe reaction mixture was concentrated under reduced pressure
- customthe residue was purified by chromatography (methylene chloride/hexanes 2:3 to 1:0)