N-Iodosuccinimide → 7-Iodo-4-(trifluoromethyl)-1H-indole-2,3-dione
反応式
[F:1][C:2]([F:15])([F:14])[C:3]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:4]=1[C:5](=[O:13])[C:6](=[O:12])[NH:7]2.[I:16]N1C(=O)CCC1=O>OS(O)(=O)=O>[I:16][C:9]1[CH:10]=[CH:11][C:3]([C:2]([F:1])([F:14])[F:15])=[C:4]2[C:8]=1[NH:7][C:6](=[O:12])[C:5]2=[O:13]参加物
4
反応条件
- 温度
- 40 °C
実験手順
A mixture of 4-trifluoromethylisatin (450 mg, 2.09 mmol) and N-iodosuccinimide (800 mg, 3.72 mmol) in conc. H2SO4 (5 mL) was stirred for 6 h at 40° C. and poured into crushed ice. The mixture was extracted with ethyl acetate and the extracts were washed with aqueous Na2SO3, dried over MgSO4, and concentrated. The residue was purified by silica gel column chromatography with 3:1 hexane/ethyl acetate to give the title compound (296 mg, 42%).
後処理
- additionpoured
- custominto crushed ice
- extractionThe mixture was extracted with ethyl acetate
- washthe extracts were washed with aqueous Na2SO3
- dry with materialdried over MgSO4
- concentrationconcentrated
- customThe residue was purified by silica gel column chromatography with 3:1 hexane/ethyl acetate
出典と根拠
- ORDレコード
- ord-200d528cbf4d4f4faa879521d7acd9e1
- 出典データセット
- uspto-grants-2003_06
- 特許番号
- US06576656B1
反応ノート
読み込み中…