2-Chloro-3-nitrobenzoic acid → (2-Chloro-3-nitrophenyl)methanol
反応式
[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4](O)=[O:5]>C1COCC1.O>[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][CH:8]=[CH:7][C:3]=1[CH2:4][OH:5]参加物
4
実験手順
10.0 g (49.61 mmol) of 2-chloro-3-nitrobenzoic acid are initially charged in 50 ml of THF. With ice cooling, 104 ml of 1M borane/THF complex are added, and the mixture is stirred at RT overnight. At 0° C., the mixture is carefully hydrolyzed using water. After the evolution of gas has ceased, the mixture is diluted with 500 ml of water and the aqueous phase is extracted three times with in total 500 ml of ethyl acetate. The organic phase is washed with saturated sodium chloride solution and dried over magnesium sulfate. The solvent is then removed under reduced pressure using a rotary evaporator. This gives 9.20 g (98% of theory) of the title compound.
後処理
- additionWith ice cooling, 104 ml of 1M borane/THF complex are added
- customAt 0° C.
- extractionthe aqueous phase is extracted three times with in total 500 ml of ethyl acetate
- washThe organic phase is washed with saturated sodium chloride solution
- dry with materialdried over magnesium sulfate
- customThe solvent is then removed under reduced pressure
- customa rotary evaporator
出典と根拠
- ORDレコード
- ord-5a88544691724218a8b2aa39388aa6b3
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07732477B2
反応ノート
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