Water → (3-TERT-BUTOXY-PHENYL)-METHANOL
反応式
[C:1]([O:5][C:6]1[CH:7]=[C:8]([CH:14]=[CH:15][CH:16]=1)[C:9](OCC)=[O:10])([CH3:4])([CH3:3])[CH3:2].[H-].[Al+3].[Li+].[H-].[H-].[H-].O>O1CCCC1>[C:1]([O:5][C:6]1[CH:7]=[C:8]([CH:14]=[CH:15][CH:16]=1)[CH2:9][OH:10])([CH3:4])([CH3:2])[CH3:3]参加物
5
実験手順
To a solution of ethyl 3-tert-butyloxybenzoate (16.7 g, 80 mmol) in tetrahydrofuran (100 ml) was added lithium aluminum hydride (4.55 g, 120 mmol) by small portions under ice-cooling. The mixture was stirred at room temperature for 1 hr. and water (10 ml) was added under ice-cooling to allow decomposition. Insoluble material was filtered off and the solvent was evaporated under reduced pressure. The residue was purified by silica gel chromatography (hexane:ethyl acetate=3:1-2:1) to give the objective substance (12.8 g, 88%) as an oil.
後処理
- temperaturecooling
- temperaturecooling
- filtrationInsoluble material was filtered off
- customthe solvent was evaporated under reduced pressure
- customThe residue was purified by silica gel chromatography (hexane:ethyl acetate=3:1-2:1)
- customto give the objective substance (12.8 g, 88%) as an oil
出典と根拠
- ORDレコード
- ord-b1dd10a15552419eb20ef2a9886c4f9e
- 出典データセット
- uspto-grants-2006_01
- 特許番号
- US06982348B2
反応ノート
読み込み中…