反応式
[C:1]([C:5]1[CH:20]=[CH:19][C:8]([O:9][CH2:10][CH2:11][C:12](OCCCC)=[O:13])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[H-].[Al+3].[Li+].[H-].[H-].[H-]>CCOCC>[C:1]([C:5]1[CH:20]=[CH:19][C:8]([O:9][CH2:10][CH2:11][CH2:12][OH:13])=[CH:7][CH:6]=1)([CH3:4])([CH3:2])[CH3:3]参加物
4
反応条件
- 温度
- -5 °C
実験手順
This ester 21.0 g was dissolved in 500 ml dry ether and cooled to -5° C. in an ice/acetone bath. To the cold solution was added, cautiously, a slurry of 3.5 g lithium aluminum hydride in 100 ml dry ether. After one hour the excess lithium aluminum hydride was destroyed by the cautious addition of 200 ml ethyl acetate, then 50 ml water. The solution was filtered and the filtrate partitioned between 200 ml ether-200 ml water. The organic layer was removed, dried, and evaporated to a yellow oil which was vacuum distilled (116° C./0.35 mm) over potassium carbonate to a clear colorless oil, 3-p-t-butylphenoxypropanol, 10.1 g (64%).
後処理
- additionTo the cold solution was added
- customAfter one hour the excess lithium aluminum hydride was destroyed by the cautious addition of 200 ml ethyl acetate
- filtrationThe solution was filtered
- customthe filtrate partitioned between 200 ml ether-200 ml water
- customThe organic layer was removed
- customdried
- customevaporated to a yellow oil which
- distillationdistilled (116° C./0.35 mm) over potassium carbonate to a clear colorless oil, 3-p-t-butylphenoxypropanol, 10.1 g (64%)
出典と根拠
- ORDレコード
- ord-ecbfde36926647cf954d8fa5ef59a520
- 出典データセット
- uspto-grants-1989_03
- 特許番号
- US04816491
関連ノート
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