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Water → 5,7-dichloro-2,4-dihydro-1H-3,1-benzoxazine-2,4-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 4,6-Dichloroisatin | HCID 251908 | — |
| 触媒 | chromium (VI) trioxide | HCID 10219390 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 5,7-dichloro-2,4-dihydro-1H-3,1-benzoxazine-2,4-dione | HCID 12363215 | — |
反応手順
To a suspension of 4,6-dichloroindolin-2,3-dione (5.95 g) in acetic acid (95 ml) was added chromium trioxide (16 g) over a period of 15 minutes at 60° C. with stirring and the mixture was stirred at 70°-75° C. for 1 hour. After cooling, the reaction mixture was poured into water (360 ml) and the resulting precipitates were collected by filtration. The filtrate was extracted with ethyl acetate. The extract was washed with water and dried. Removal of the solvent gave a residue, which was combined with the precipitates. Recrystallization from isopropyl ether gave 5,7-dichloro-2H-3,1-benzoxazine-2,4(1H)-dione (2.85 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04734419 |
| 出典データセット | uspto-grants-1988_03 |
| ORD ID | ord-96b79913e52e4204b7065cc2cf9372a3 |
| 出典メモ | uspto-grants-1988_03 |