Methanol → 4-Bromo-3-fluoro-2-methylbenzoic acid
反応式
[Br:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[F:11].O.[CH3:13]O>S(=O)(=O)(O)O>[CH3:13][C:4]1[C:3]([F:11])=[C:2]([Br:1])[CH:10]=[CH:9][C:5]=1[C:6]([OH:8])=[O:7]参加物
5
実験手順
4-Bromo-3-fluorobenzoic acid (WAKO, 1.0 g) was dissolved in methanol (10 mL), followed by addition of concentrated sulfuric acid (10 drops). The mixture was refluxed for three hours. After cooling to room temperature, water was added and the extraction was carried out with ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure to obtain the target compound (618 mg).
後処理
- temperatureThe mixture was refluxed for three hours
- extractionthe extraction
- washThe organic layer was washed with brine
- dry with materialdried over anhydrous sodium sulfate
- distillationthe solvent was distilled off under reduced pressure
出典と根拠
- ORDレコード
- ord-299044bc3ba543eeba9f203ba863f82b
- 出典データセット
- uspto-grants-2011_10
- 特許番号
- US08039514B2
反応ノート
読み込み中…