Sodium borohydride → (2-Ethoxypyridin-4-yl)methanol
反応式
[BH4-].[Na+].[CH2:3]([O:5][C:6]1[CH:11]=[C:10]([C:12](OCC)=[O:13])[CH:9]=[CH:8][N:7]=1)[CH3:4]>C(O)C.ClCCl>[CH2:3]([O:5][C:6]1[CH:11]=[C:10]([CH2:12][OH:13])[CH:9]=[CH:8][N:7]=1)[CH3:4]参加物
5
実験手順
0.508 g of sodium borohydride is added portionwise to a solution of 0.524 g of ethyl 2-ethoxypyridine-4-carboxylate in 5.2 ml of ethanol, under an inert atmosphere of argon at a temperature in the region of 0° C. The reaction mixture is refluxed with stirring for 3 hours and then concentrated to dryness under reduced pressure. The residue thus obtained is taken up in 50 ml of dichloromethane and then washed with 50 ml of water. The organic phase is dried over magnesium sulfate, filtered and then concentrated to dryness under reduced pressure. 0.310 g of 2-ethoxy-4-(hydroxymethyl)pyridine is thus obtained.
後処理
- temperatureThe reaction mixture is refluxed
- concentrationconcentrated to dryness under reduced pressure
- customThe residue thus obtained
- washwashed with 50 ml of water
- dry with materialThe organic phase is dried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated to dryness under reduced pressure
出典と根拠
- ORDレコード
- ord-e444a2ea74b64ab4bff654908f006f6f
- 出典データセット
- uspto-grants-2008_04
- 特許番号
- US07354933B2
反応ノート
読み込み中…