p-Toluenesulfonic acid → Ethyl 3-methoxy-4-methylphenylacetate
反応式
[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]参加物
4
実験手順
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.
後処理
- 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)
出典と根拠
- ORDレコード
- ord-825aa86bdae84b0cac58a6d2d8eb79cb
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09115072B2
反応ノート
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