Thionyl Chloride → HCID 86710737、化合物
反応式
[NH2:1][C:2]1[N:7]=[C:6]2[N:8]([CH3:25])[N:9]=[C:10]([C:11]3[C:12]([O:23][CH3:24])=[CH:13][C:14]([O:21][CH3:22])=[C:15]([S:17](O)(=[O:19])=[O:18])[CH:16]=3)[C:5]2=[CH:4][N:3]=1.S(Cl)([Cl:28])=O>>[NH2:1][C:2]1[N:7]=[C:6]2[N:8]([CH3:25])[N:9]=[C:10]([C:11]3[C:12]([O:23][CH3:24])=[CH:13][C:14]([O:21][CH3:22])=[C:15]([S:17]([Cl:28])(=[O:19])=[O:18])[CH:16]=3)[C:5]2=[CH:4][N:3]=1参加物
3
反応条件
- 温度
- 120 °C
実験手順
5-(6-Amino-1-methyl-1H-pyrazolo[3,4-d]pyrimidin-3-yl)-2,4-dimethoxy-benzenesulfonic acid (Example 113) (629 mg, 1.72 mmol) is suspended in thionyl chloride (25 ml), the reaction mixture is heated to 120° C. for 5 hours then stood overnight at room temperature. The resulting precipitate is removed by filtration, the filtrate is concentrated in vacuo and the resulting residue is azeotroped with toluene to afford the title compound as a solid.
後処理
- customThe resulting precipitate is removed by filtration
- concentrationthe filtrate is concentrated in vacuo
- custom