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
PROCEDURE
实验过程
A mixture of toluene (370 mL) and water (70 mL) was degassed with nitrogen for 30 minutes. A mixture of cesium carbonate (102.6 g, 315 mmol), 4-bromo-2,3,5,6-tetrafluoro-benzoic acid methyl ester (30.0 g, 105 mmol), phenyl boronic acid (19.26 g, 157 mmol) and tetrakis triphenyl phosphene palladium(0) (11.5 g, 9.9 mmol) were added to the above degassed water/toluene mixture. The reaction mixture was refluxed overnight. After the reaction is completed, it was cooled to room temperature and extracted with ethyl acetate. The combined organic layers were dried over sodium sulphate and concentrated. The resulting residue was purified by column chromatography using 5% ethyl acetate in hexane to obtain the title compound (26.5 g, 88.6%).
WORKUP
后处理
- customwas degassed with nitrogen for 30 minutes
- additionwere added to the
- customabove degassed water/toluene mixture
- temperatureThe reaction mixture was refluxed overnight
- extractionextracted with ethyl acetate
- dry with materialThe combined organic layers were dried over sodium sulphate
- concentrationconcentrated
- customThe resulting residue was purified by column chromatography