(5-Fluoro-2-methoxypyridin-3-yl)methanol → 5-Fluoro-2-methoxynicotinaldehyde
反応式
[F:1][C:2]1[CH:3]=[C:4]([CH2:10][OH:11])[C:5]([O:8][CH3:9])=[N:6][CH:7]=1>C(OCC)(=O)C.[O-2].[Mn+4].[O-2]>[F:1][C:2]1[CH:3]=[C:4]([CH:10]=[O:11])[C:5]([O:8][CH3:9])=[N:6][CH:7]=1参加物
4
実験手順
To (5-fluoro-2-methoxy-pyridin-3-yl)-methanol (36, 8 g, 50.9 mmol) in 300 mL of ethyl acetate, manganese(IV) oxide (39.8 g, 458 mmol) was added and the mixture stirred at room temperature overnight. The reaction mixture was filtered through celite, and the celite bed rinsed with ethyl acetate. The filtrate was concentrated under vacuum, then passed through a plug of silica, eluting with 50% ethyl acetate in heptane to provide the desired compound as a light yellow solid (37, 4.5 g, 29.0 mmol, 57.0% yield).
後処理
- filtrationThe reaction mixture was filtered through celite
- washthe celite bed rinsed with ethyl acetate
- concentrationThe filtrate was concentrated under vacuum
- washeluting with 50% ethyl acetate in heptane
出典と根拠
- ORDレコード
- ord-973f28eabc2548f0814f563d2ede27d0
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09096593B2
反応ノート
読み込み中…