p-Toluenesulfonic acid → Ethyl 3-methoxy-4-methylphenylacetate
반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:10][C:11]([OH:13])=[O:12])[CH:6]=[CH:7][C:8]=1[CH3:9].[CH3:14][C:15]1C=CC(S(O)(=O)=O)=CC=1>C(O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])[CH:6]=[CH:7][C:8]=1[CH3:9]참가 물질
4
실험 절차
To a stirred solution of 2-(3-methoxy-4-methylphenyl)acetic acid (Step A, 4.64 g, 25.7 mmol) in ethanol (100 ml) was added p-TsOH (0.7 g, 3.7 mmol) at room temperature under argon and the reaction mixture was refluxed for 12 hours or until all the starting material is consumed, concentrated, diluted in EtOAc and washed with 0.1N HCl, brine, dried over Na2SO4, filtered, concentrated and purified by flash chromatography on a silica gel column (hexane:ethyl acetate, 2:1) to give the title compound.
후처리
- temperaturethe reaction mixture was refluxed for 12 hours or until all the starting material
- customis consumed
- concentrationconcentrated
- additiondiluted in EtOAc
- washwashed with 0.1N HCl, brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- custompurified by flash chromatography on a silica gel column (hexane:ethyl acetate, 2:1)
출처 및 근거
- ORD 기록
- ord-825aa86bdae84b0cac58a6d2d8eb79cb
- 출처 데이터셋
- uspto-grants-2015_08
- 특허 번호
- US09115072B2
반응 노트
불러오는 중…