Hydroxylamine HCl → 2-Chloro-3-hydroxybenzonitrile
반응식
[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]참가 물질
5
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-ada5673d3bfe4b2b954acd2604a1bd63
- 출처 데이터셋
- uspto-grants-2009_07
- 특허 번호
- US07557131B2
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