Hydrogen Peroxide → 2-(4-Chlorophenyl)-1,2,3,4-tetrahydro[1]benzothiopyrano[4,3-c]pyrazol-3-one-5-oxide
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12](=[O:13])[C:11]3[CH2:14][S:15][C:16]4[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=4[C:10]=3[NH:9]2)=[CH:4][CH:3]=1.[OH:22]O>C(O)(=O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]2[C:12](=[O:13])[C:11]3[CH2:14][S:15](=[O:22])[C:16]4[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=4[C:10]=3[NH:9]2)=[CH:6][CH:7]=1参加物
4
反応条件
- 温度
- 0 °C
実験手順
In a 50 ml. round bottom flask under nitrogen was placed 2-(p-chlorophenyl)-1,2,3,4-tetrahydro[1]benzothiopyrano[4,3-c]pyrazole-3-one (0.5 g., 0.0016 mole) 8.33 ml. of glacial acetic acid and 3 ml. of 30% hydrogen peroxide. After stirring at 0° C., for 3.5 hours, the resulting solid was removed by filtration, washed with glacial acetic acid and dried in vacuo over phosphorous pentoxide to afford product, m.p. 193° C. (dec.). Weight 0.42 g. (80%). A second crop (0.4 g., 8%) was obtained from mother liquors.