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Hydroxylamine HCl → 2-Chloro-3-hydroxybenzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydroxylamine HCl | HCID 21645 | — |
| 反応物 | 2-Chloro-3-hydroxybenzaldehyde | HCID 593376 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-Chloro-3-hydroxybenzonitrile | HCID 21436545 | — |
反応手順
A mixture of 2-chloro-3-hydroxybenzaldehyde [(2 g, 12.8 mmol) WO 2005007633, p34] and hydroxyl ammonium chloride (1.33 g, 19.6 mmol) in acetic acid (20 mL) was heated under reflux for 2 hours. The reaction mixture was then cooled to room temperature and partitioned between diethyl ether and water. The organic layer was separated, washed with brine, dried over magnesium sulfate and concentrated in vacuo to give a white solid. The solid was then dissolved in ethyl acetate washed with water and brine, dried over magnesium sulfate and concentrated in vacuo to afford the title compound as a solid in quantitative yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07557131B2 |
| 出典データセット | uspto-grants-2009_07 |
| ORD ID | ord-ada5673d3bfe4b2b954acd2604a1bd63 |
| 出典メモ | uspto-grants-2009_07 |