関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Chloral Hydrate | HCID 2707 | — |
| 反応物 | Sodium Sulfate | HCID 24436 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | 4-Bromo-2-ethylaniline | HCID 2801283 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | N-(4-Bromo-2-ethyl-phenyl)-2-hydroxyimino-acetamide | HCID 86041545 | 46% |
反応手順
To a suspension of 4-bromo-2-ethylaniline (50.0 g, 250 mmol) in water (1000 mL) was added concentrated hydrochloric acid (25 mL), sodium sulfate (220 g), and hydroxylamine hydrochloride (56.25 g), followed by addition of chloral hydrate (44.0 g). The reaction mixture was heated to 90° C. using an oil bath for 1 hour. After cooling down to room temperature, it was extracted with ethyl acetate. Extract was dried over magnesium sulfate and concentrated under reduced pressure to give the title compound (31.1 g, 46% yield). 1H NMR (DMSO-d6) δ 12.24 (s, 1H), 9.56 (s, 1H), 7.68 (s, 1H), 7.41 (m, 3H), 2.58 (q, 2H), 1.11 (t, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07446122B2 |
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| 出典データセット | uspto-grants-2008_11 |
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| ORD ID | ord-1926690a1aa74c89addfd329923aee6a |
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| 出典メモ | uspto-grants-2008_11 |
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