Potassium Hydroxide → 2-Chloro-3,5-Dimethoxyaniline
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[OH-].[K+].[Cl:3][C:4]1[C:9]([O:10][CH3:11])=[CH:8][C:7]([O:12][CH3:13])=[CH:6][C:5]=1[NH:14]C(=O)C>CCO.O>[Cl:3][C:4]1[C:9]([O:10][CH3:11])=[CH:8][C:7]([O:12][CH3:13])=[CH:6][C:5]=1[NH2:14]참가 물질
5
실험 절차
Potassium hydroxide (2.19 g, 39.18 mmol) was added to a solution of N-(2-chloro-3,5-dimethoxyphenyl)acetamide (1.8 g, 7.837 mmol) in EtOH (100 mL) and water (10 mL) and the reaction mixture heated to reflux for 12 h. Excess EtOH was removed under reduced pressure to obtain a residue. The residue was then partitioned between water and diethyl ether. The organic layer was separated, dried over sodium sulfate, filtered and concentrated under vacuum to afford the title compound (1.2 g, 82% of yield) as a white solid. 1HNMR (CDCl3, 300 MHz): δ 5.97 (s, 2H), 4.08 (brs, 2H), 3.84 (s, 3H), 3.75 (s, 3H); MS (ESI): 188.1 [M+H]+.
후처리
- temperaturethe reaction mixture heated
- temperatureto reflux for 12 h
- customExcess EtOH was removed under reduced pressure
- customto obtain a residue
- customThe residue was then partitioned between water and diethyl ether
- customThe organic layer was separated
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated under vacuum
출처 및 근거
- ORD 기록
- ord-e54c098ae5e44c79abbbc706661fc090
- 출처 데이터셋
- uspto-grants-2016_09
- 특허 번호
- US09434697B2
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