Methanol → 2-Fluoro-1-methoxy-5-methyl-3-(methylsulfinyl)benzene
反応式
[F:1][C:2]1[C:7]([S:8][CH3:9])=[CH:6][C:5]([CH3:10])=[CH:4][C:3]=1[O:11][CH3:12].C[OH:14]>O>[F:1][C:2]1[C:7]([S:8]([CH3:9])=[O:14])=[CH:6][C:5]([CH3:10])=[CH:4][C:3]=1[O:11][CH3:12]参加物
4
実験手順
To a mixture of 2-fluoro-1-methoxy-5-methyl-3-(methylsulfanyl)benzene (557.4 mg), MeOH (20 mL) and water (4 mL) was added NaIO4 (960 mg) at 0° C. The mixture was stirred at room temperature over weekend. The mixture was diluted with water. The precipitate was filtered off, and the filtrate was extracted with EtOAc. The organic layer was washed with brine, dried over MgSO4, filtered and concentrated in vacuo. The residue was purified by silica gel column chromatography (EtOAc/hexane) to give the title compound (486 mg).
後処理
- filtrationThe precipitate was filtered off
- extractionthe filtrate was extracted with EtOAc
- washThe organic layer was washed with brine
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe residue was purified by silica gel column chromatography (EtOAc/hexane)
出典と根拠
- ORDレコード
- ord-5925f71deda44fc398619b779216804f
- 出典データセット
- uspto-grants-2016_01
- 特許番号
- US09238639B2
反応ノート
読み込み中…