Dimethylformamide → 3-(Difluoromethoxy)benzaldehyde
反応式
[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]参加物
6
反応条件
- 温度
- 100 °C
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-de68ac8e0ea145089587f8be7584033d
- 出典データセット
- uspto-grants-2013_10
- 特許番号
- US08557992B2
反応ノート
読み込み中…