Hydrogen Peroxide → 6-Chloro-5-fluoroisatoic acid anhydride
반응식
[Cl:1][C:2]1[C:10]([F:11])=[CH:9][CH:8]=[C:7]2[C:3]=1[C:4](=[O:13])[C:5](=[O:12])[NH:6]2.S(=O)(=O)(O)[OH:15].OO>C(O)(=O)C>[Cl:1][C:2]1[C:10]([F:11])=[CH:9][CH:8]=[C:7]2[NH:6][C:5](=[O:15])[O:12][C:4](=[O:13])[C:3]=12참가 물질
5
실험 절차
7.8 g (0.039 mol) of 4-chloro-5-fluoro-isatin are suspended in 50 ml of 100 percent acetic acid, treated with 0.25 ml of concentrated sulphuric acid and then 4.4 ml (0.043 mol) of 30 percent hydrogen peroxide are added dropwise thereto. The mixture is subsequently heated to 70° for 2.5 hours, then cooled to 10° and filtered. The crude product is recrystallized from acetone/hexane, there being obtained 6-chloro-5-fluoro-isatoic acid anhydride of melting point 275°-278° (decomposition).
후처리
- temperatureThe mixture is subsequently heated to 70° for 2.5 hours
- temperaturecooled to 10°
- filtrationfiltered
- customThe crude product is recrystallized from acetone/hexane, there
출처 및 근거
- ORD 기록
- ord-237ba3d8d381429797a0ca0eda6b6169
- 출처 데이터셋
- uspto-grants-1984_12
- 특허 번호
- US04489003
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