Sodium borohydride → 2,2-Difluoro-2-(pyridin-4-yl)-ethanol
反応式
[N:1]1[CH:6]=[CH:5][C:4]([C:7]([F:14])([F:13])[C:8](OCC)=[O:9])=[CH:3][CH:2]=1.[BH4-].[Na+]>C(O)C>[F:14][C:7]([F:13])([C:4]1[CH:5]=[CH:6][N:1]=[CH:2][CH:3]=1)[CH2:8][OH:9]参加物
4
実験手順
To a solution of ethyl pyridin-4-yl-difluoroacetate (0.59 g) prepared in (1) in ethanol (10 mL) was added NaBH4 (0.11 g) at 0° C. The reaction mixture was stirred at RT for 2 hr. The solvent was removed under reduced pressure. Water was added to the residue and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous NaHCO3, and then dried over MgSO4. The solvent was removed under reduced pressure. The residue was purified by silica gel chromatography (Developing solvent: ethyl acetate) to give the title compound (0.082 g, 1%).
後処理
- customThe solvent was removed under reduced pressure
- additionWater was added to the residue
- extractionthe mixture was extracted with ethyl acetate
- washThe organic layer was washed with saturated aqueous NaHCO3
- dry with materialdried over MgSO4
- customThe solvent was removed under reduced pressure
- customThe residue was purified by silica gel chromatography (Developing solvent: ethyl acetate)
出典と根拠
- ORDレコード
- ord-f6aefafcc0f24584a3a37d4800df952b
- 出典データセット
- uspto-grants-2014_07
- 特許番号
- US08765739B2
反応ノート
読み込み中…