Dimethylformamide → 3-(Difluoromethoxy)benzaldehyde
반응식
[O:1]=[C:2]1[CH:7]=[C:6]([CH:8]=[O:9])[CH:5]=[CH:4]N1.Cl[C:11]([F:16])([F:15])C([O-])=O.[Na+].[CH3:18]N(C=O)C>C(#N)C.C(OCC)(=O)C>[F:15][CH:11]([F:16])[O:1][C:2]1[CH:7]=[C:6]([CH:5]=[CH:4][CH:18]=1)[CH:8]=[O:9]참가 물질
6
반응 조건
- 온도
- 100 °C
실험 절차
To a solution of 2-oxo-1,2-dihydropyridine-4-carbaldehyde (1.72 g, 11.3 mmol) in 25 mL of acetonitrile was added sodium chlorodifluoroacetate (0.925 g, 7.51 mmol). The reaction was heated to reflux under an atmosphere of nitrogen for 15 h, and then DMF (3 mL) was added. The mixture was heated to 100° C. for 3 d, cooled to rt, and diluted with ethyl acetate. The organic solution was washed with brine, dried over sodium sulfate, filtered, and concentrated in vacuo to provide 3-(difluoromethoxy)benzaldehyde.
후처리
- temperatureThe reaction was heated
- temperatureto reflux under an atmosphere of nitrogen for 15 h
- temperaturecooled to rt
- washThe organic solution was washed with brine
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
출처 및 근거
- ORD 기록
- ord-de68ac8e0ea145089587f8be7584033d
- 출처 데이터셋
- uspto-grants-2013_10
- 특허 번호
- US08557992B2
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