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Acetic Acid → 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 | Acetic Acid | HCID 176 | — |
| 反応物 | 4,6-Dichloroisatin | HCID 251908 | — |
| 触媒 | chromium (VI) trioxide | HCID 10219390 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Acetic Anhydride | HCID 7918 | — |
| 生成物 | 5,7-dichloro-2,4-dihydro-1H-3,1-benzoxazine-2,4-dione | HCID 12363215 | 72% |
反応手順
To a stirred solution of 4,6-dichloro-1H-indole-2,3-dione (5.00 g, 23.2 mM) in acetic acid (21 mL) and acetic anhydride (21 mL) at 80° C. was added in small portions chromium trioxide (4.12 g, 41.3 mM). The temperature of the reaction mixture was maintained between 80°-90° C. during the addition of the chromium trioxide. After the addition was complete, the reaction mixture was diluted with water (100 mL) and then filtered to separate the precipitated solids. The solids were washed thoroughly with water and then dried to obtain the title compound as a yellow solid (4.13 g, 72%); MS(CI): 232 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05733910 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-62f911c33ec34c2dbe633593e1d5ee82 |
| 出典メモ | uspto-grants-1998_03 |