Hydrochloric Acid → [2,6-Difluoro-4-(1-hydroxy-1-methyl-ethyl)-phenyl]-acetaldehyde
反応式
[F:1][C:2]1[CH:3]=[C:4]([C:13]([OH:16])([CH3:15])[CH3:14])[CH:5]=[C:6]([F:12])[C:7]=1[CH:8]=[CH:9][O:10]C.Cl>CC(C)=O>[F:1][C:2]1[CH:3]=[C:4]([C:13]([OH:16])([CH3:14])[CH3:15])[CH:5]=[C:6]([F:12])[C:7]=1[CH2:8][CH:9]=[O:10]参加物
4
実験手順
A solution of 2-{3,5-difluoro-4-[2-methoxyvinyl]phenyl}propan-2-ol (5.0 g, 22 mmol) in acetone (25 mL) was added dropwise to 4 M aqueous hydrochloric acid (25 mL, 100 mmol) with ice-water cooling, keeping the temperature below 10° C. Then the mixture was stirred at room temperature for six hours. The resulting mixture was extracted with ethyl acetate (2×) and the combined organic phases were washed with saturated aqueous sodium bicarbonate and brine. The organic layer was then dried and concentrated in vacuo to afford the title compound.
後処理
- customthe temperature below 10° C
- extractionThe resulting mixture was extracted with ethyl acetate (2×)
- washthe combined organic phases were washed with saturated aqueous sodium bicarbonate and brine
- customThe organic layer was then dried
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-61d0ccc73edd4c0d8a1fa039bb5e8d42
- 出典データセット
- uspto-grants-2013_02
- 特許番号
- US08367706B2
反応ノート
読み込み中…