反応式
[CH3:1][S:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][C:11](O)=[O:12])=[CH:5][CH:4]=1.O1CCCC1.B.O.Cl>O1CCCC1>[CH3:1][S:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][CH2:11][OH:12])=[CH:5][CH:4]=1参加物
実験手順
3-(4-Methylsulfanylphenyl)propionic acid (1.00 g) was dissolved in tetrahydrofuran (20 ml), and a tetrahydrofuran-borane.tetrahydrofuran solution (1 mol/l, 6.42 ml) was added dropwise to the mixture under ice-cooling. The mixture was stirred under ice-cooling for 30 min, and further at room temperature for 1 hr. Water was added to the reaction mixture, and 1 mol/l aqueous hydrochloric acid solution was added. The mixture was extracted with ethyl acetate, washed with water, saturated aqueous sodium hydrogen carbonate solution and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel chromatography to give the object product (940 mg) as a colorless oil.
後処理
- temperaturecooling
- temperaturecooling for 30 min
- additionwas added
- extractionThe mixture was extracted with ethyl acetate
- washwashed with water, saturated aqueous sodium hydrogen carbonate solution and saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- customThe solvent was evaporated under reduced pressure
- customThe residue was purified by silica gel chromatography
出典と根拠
- ORDレコード
- ord-dc64a8753add475fb3266aac59b62ac0
- 出典データセット
- uspto-grants-2012_03
- 特許番号
- US08129361B2
関連ノート
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