Methanol → Methyl 2-(3-fluoro-4-methylphenyl)acetate
反応式
[F:1][C:2]1[CH:3]=[C:4]([CH2:9][C:10]([OH:12])=[O:11])[CH:5]=[CH:6][C:7]=1[CH3:8].S(=O)(=O)(O)O.[CH3:18]O>>[F:1][C:2]1[CH:3]=[C:4]([CH2:9][C:10]([O:12][CH3:18])=[O:11])[CH:5]=[CH:6][C:7]=1[CH3:8]参加物
4
反応条件
- 温度
- 85 °C
実験手順
(3-Fluoro-4-methylphenyl)acetic acid (105.3 g) was dissolved in methanol (740 ml) and concentrated sulfuric acid (9.9 ml) was added. The mixture was stirred at 85° C. for 1 hr. The reaction mixture was cooled to room temperature, and concentrated under reduced pressure. Water was added to the obtained residue and the mixture was extracted with ethyl acetate (1 L). The organic layer was washed successively with water, aqueous sodium hydrogencarbonate solution, water and saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to give the title compound (114.2 g).
後処理
- temperatureThe reaction mixture was cooled to room temperature
- concentrationconcentrated under reduced pressure
- additionWater was added to the obtained residue
- extractionthe mixture was extracted with ethyl acetate (1 L)
- washThe organic layer was washed successively with water, aqueous sodium hydrogencarbonate solution, water and saturated brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-55ff220c72f946da93332ae138e336a0
- 出典データセット
- uspto-grants-2007_12
- 特許番号
- US07304174B2
反応ノート
読み込み中…