反応式
F[C:2]1[C:3]([N+:8]([O-:10])=[O:9])=[N:4][CH:5]=[CH:6][CH:7]=1.[CH2:11]([C:13]1[CH:18]=[CH:17][C:16]([OH:19])=[C:15]([O:20][CH3:21])[CH:14]=1)[CH3:12].[OH-].[K+]>C(#N)C>[CH2:11]([C:13]1[CH:18]=[CH:17][C:16]([O:19][C:2]2[C:3]([N+:8]([O-:10])=[O:9])=[N:4][CH:5]=[CH:6][CH:7]=2)=[C:15]([O:20][CH3:21])[CH:14]=1)[CH3:12]参加物
5
反応条件
- 温度
- 80 °C
実験手順
To a stirred solution of 3-Fluoro 2-nitro pyridine (1.6 g, 0.01126 mol) in dry Acetonitrile (20 ml) was added 4-Ethyl-2-methoxy phenol (1.71 g, 11.3 mmol) in dry acetonitrile (10 ml) followed by potassium hydroxide (0.696 g, 12.4 mmol). The reaction mixture was heated to 80° C. and maintained for 2 hours. The solvent was evaporated and taken in ethyl acetate (200 ml). The organic layer was washed with water followed by brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure to give 2.6 g of crude product purified by column chromatography (5% Ethyl acetate in Petroleum ether) to yield: 1.75 g (56%) of title compound.
後処理
- temperaturemaintained for 2 hours
- customThe solvent was evaporated
- washThe organic layer was washed with water
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-0134fb5f56ae4a8e9368241693265e86
- 出典データセット
- uspto-grants-2016_04
- 特許番号
- US09309179B2
関連ノート
読み込み中…