HRID17884
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 150 °C
PROCEDURE
实验过程
3-(3-Benzyloxyphenyl)-3-oxopropionate ethyl ester (174.42 g, 584.47 mmol) was dissolved in m-xylene and the reaction mixture was refluxed while stirring for 30 min at 150° C. Then, isopropylamine (38 g, 642.92 mmol) was added dropwise to the mixture. After stirring and refluxing for 24 hours at room temperature, the organic layer was extracted with saturated sodium chloride and ethyl acetate, dried over anhydrous magnesium sulfate, concentrated, and resulting residue was purified by column chromatography (ethyl acetate:hexane=1:2) to obtain 2-(3-benzyloxybenzoyl)-N-isopropyl-3-phenylacryl amide (127.13 g, yield 70%) as yellow oil.
WORKUP
后处理
- temperaturethe reaction mixture was refluxed
- stirringAfter stirring
- temperaturerefluxing for 24 hours at room temperature
- extractionthe organic layer was extracted with saturated sodium chloride and ethyl acetate
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated
- customresulting residue
- customwas purified by column chromatography (ethyl acetate:hexane=1:2)