関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | N-(4-Bromo-2-ethyl-phenyl)-2-hydroxyimino-acetamide | HCID 86041545 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-Bromo-7-ethylindoline-2,3-dione | HCID 8033813 | 74% |
反応手順
To a solution of sulfuric acid (100 mL) and water (10 mL) at 80° C. (oil bath) was added N-(4-bromo-2-ethyl-phenyl)-2-hydroximino-acetoamide (61.0 g, 225 mmol) in small portions over 20 minutes. The reaction mixture was heated at 80° C. (oil bath) for 15 minutes. After cooling to room temperature, ice-water (500 mL) was added and the mixture was extracted with ethyl acetate. Extracts were washed with saturated sodium bicarbonate solution, dried over magnesium sulfate, and concentrated under reduced pressure to give the title compound (42.3 g, 74% yield). 1H NMR (DMSO-d6) δ 8.87 (s, 1H), 7.75 (d, 1H), 7.71 (d, 1H), 2.75 (q, 2H), 1.44 (t, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07314886B2 |
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| 出典データセット | uspto-grants-2008_01 |
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| ORD ID | ord-38f1b47e28114101bfcce833626d4d29 |
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| 出典メモ | uspto-grants-2008_01 |
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