4-(5-fluoropyridin-2-yl)-N-methoxy-N-methylbenzamide → 1-(4-(5-Fluoropyridin-2-yl)phenyl)ethanone
反応式
[CH3:1][Mg]Br.[F:4][C:5]1[CH:6]=[CH:7][C:8]([C:11]2[CH:22]=[CH:21][C:14]([C:15](N(OC)C)=[O:16])=[CH:13][CH:12]=2)=[N:9][CH:10]=1>O1CCCC1>[F:4][C:5]1[CH:6]=[CH:7][C:8]([C:11]2[CH:22]=[CH:21][C:14]([C:15](=[O:16])[CH3:1])=[CH:13][CH:12]=2)=[N:9][CH:10]=1参加物
4
反応条件
- 温度
- 0 °C
実験手順
Methylmagnesium bromide (3 M in tetrahydrofuran) (2.1 mL, 6.2 mmol) was added to a −78° C. solution of 4-(5-fluoropyridin-2-yl)-N-methoxy-N-methylbenzamide (800 mg, 3.1 mmol) in tetrahydrofuran (20 mL). After stirring at 0° C. for 30 min, the reaction mixture was quenched with methanol and saturated aqueous ammonium chloride. The organic layer was dried (magnesium sulfate) and concentrated in vacuo. Chromatography over silica eluting with 0-15% ethyl acetate/hexane afforded the title compound.
後処理
- customthe reaction mixture was quenched with methanol and saturated aqueous ammonium chloride
- dry with materialThe organic layer was dried (magnesium sulfate)
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-fb6eadfff345482abeb6415983a5f2e8
- 出典データセット
- uspto-grants-2012_06
- 特許番号
- US08193228B2
反応ノート
読み込み中…