Hydroxylamine HCl → 2-Chloro-3-hydroxybenzonitrile
反応式
[Cl:1][C:2]1[C:9]([OH:10])=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=O.[Cl-].O[NH3+:13]>C(O)(=O)C.C(OCC)(=O)C>[Cl:1][C:2]1[C:9]([OH:10])=[CH:8][CH:7]=[CH:6][C:3]=1[C:4]#[N:13]参加物
5
実験手順
A mixture of 2-chloro-3-hydroxybenzaldehyde [(2 g, 12.8 mmol) WO 2005007633, p 34] and hydroxylammonium 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.
後処理
- temperaturewas heated
- temperatureunder reflux for 2 hours
- custompartitioned between diethyl ether and water
- customThe organic layer was separated
- washwashed with brine
- dry with materialdried over magnesium sulfate
- concentrationconcentrated in vacuo
- customto give a white solid
- washwashed with water and brine
- dry with materialdried over magnesium sulfate
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-3228a409c4a9446ebecc30f3b3fc2962
- 出典データセット
- uspto-grants-2012_06
- 特許番号
- US08207198B2
反応ノート
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