Water → 2-(2-Propylimidazol-1-yl)propan-1-ol
反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([C:10]1[N:11]([CH:15]([CH3:21])[C:16](OCC)=[O:17])[CH:12]=[CH:13][N:14]=1)[CH2:8][CH3:9].O.[OH-].[Na+]>O1CCCC1>[CH2:7]([C:10]1[N:11]([CH:15]([CH3:21])[CH2:16][OH:17])[CH:12]=[CH:13][N:14]=1)[CH2:8][CH3:9]参加物
6
反応条件
- 温度
- 0 °C
実験手順
Lithium aluminum hydride (2.5 g) was suspended in tetrahydrofuran (40 ml). Ethyl 2-(2-propylimidazol-1-yl)propanate [9.2 g] in tetrahydrofuran (40 ml) was added with stirring at 0° C. The reaction was refluxed for 3 hours, cooled to 0° C., water (3 ml) was added dropwise followed by 15% sodium hydroxide (3 ml) and a further portion of water (9 ml). The suspension was filtered through solka-flok and the solvent removed under reduced pressure. Dichloromethane (50 ml) was added, the organic phase washed with brine (25 ml) dried over magnesium sulphate and the solvent removed under reduced pressure yielding the title compound as a white foam 5.4 g (67%).
後処理
- temperatureThe reaction was refluxed for 3 hours
- temperaturecooled to 0° C.
- filtrationThe suspension was filtered through solka-flok and the solvent
- customremoved under reduced pressure
- additionDichloromethane (50 ml) was added
- washthe organic phase washed with brine (25 ml)
- dry with materialdried over magnesium sulphate
- customthe solvent removed under reduced pressure
出典と根拠
- ORDレコード
- ord-3546e09500dc4a36a4942db3a2a462ea
- 出典データセット
- uspto-grants-1989_08
- 特許番号
- US04853392
反応ノート
読み込み中…