Methanol → (5-Bromo-3-fluoropyridin-2-yl)methanol
反応式
[Br:1][C:2]1[CH:3]=[C:4]([F:11])[C:5]([C:8](Cl)=[O:9])=[N:6][CH:7]=1.[BH4-].[Li+].CO>O1CCCC1>[Br:1][C:2]1[CH:3]=[C:4]([F:11])[C:5]([CH2:8][OH:9])=[N:6][CH:7]=1参加物
5
反応条件
- 温度
- 0 °C
実験手順
5-Bromo-3-fluoropyridine-2-carbonyl chloride (0.50 g, 2.1 mmol) was dissolved in tetrahydrofuran (10 mL), cooled to 0° C. and treated with lithium borohydride (1.0 mL, 2 M tetrahydrofuran solution, 2.1 mmol, 1 equiv). After stirring for 30 minutes at 0° C., the mixture was treated with methanol (2 mL) and concentrated in vacuo. The residue was purified by silica gel gradient chromatography (100:0 to 0:100; hexanes:ethyl acetate), providing the titled compound.
後処理
- concentrationconcentrated in vacuo
- customThe residue was purified by silica gel gradient chromatography (100:0 to 0:100; hexanes:ethyl acetate)
出典と根拠
- ORDレコード
- ord-27632c39ac1f41b7a8c221daf11968e7
- 出典データセット
- uspto-grants-2014_11
- 特許番号
- US08895580B2
反応ノート
読み込み中…