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
Palladium acetate (21 mg, 7 mol %) was added to a solution of 2-bromo-4-chloroanisole (300 mg, 1.4 mmol), styrene (211 mg, 2 mmol), triethylamine (13 μL, 0.1 mmol) and triphenylphosphine (50 mg, 1.9 mmol) in acetonitrile (6 mL), and the mixture was refluxed for 8 hours under argon atmosphere. After the reaction mixture was cooled to room temperature, the solvent was concentrated under reduced pressure and the obtained residue was diluted with ethyl acetate (15 mL). After the solution was washed successively with 2N hydrochloric acid, water and brine, dried over anhydrous sodium sulfate, the residue obtained by evaporation of the solvent under reduced pressure was purified by column chromatography on silica gel (n-hexane:ethyl acetate=10:1) to give the title compound (118 mg, 35.6%) as a white powder.
WORKUP
后处理
- temperaturethe mixture was refluxed for 8 hours under argon atmosphere
- concentrationthe solvent was concentrated under reduced pressure
- additionthe obtained residue was diluted with ethyl acetate (15 mL)
- washAfter the solution was washed successively with 2N hydrochloric acid, water and brine
- dry with materialdried over anhydrous sodium sulfate
- customthe residue obtained by evaporation of the solvent under reduced pressure
- customwas purified by column chromatography on silica gel (n-hexane:ethyl acetate=10:1)