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
The title compound was synthesized by referring to Chem. Lett., 2000, (7), 738. To a solution of 1-(2,4-dimethoxyphenyl)-2-(4-methoxyphenyl)ethanone (2.8 g) in acetonitrile (150 ml) were sequentially added sodium iodide (3.0 g) and cerium(III) chloride heptahydrate (5.7 g), and the solution was refluxed for 20 hours and 30 minutes. Sodium iodide (760 mg) and cerium(III) chloride heptahydrate (1.9 g) were added thereto, and the solution was further refluxed for 22 hours 30 minutes. To the reaction solution were added ethyl acetate and water, the solution was filtered through celite pad, extracted with ethyl acetate, then washed with brine, dried over anhydrous magnesium sulfate, and then filtered. The filtrate was adsorbed onto silica gel and purified by silica gel column chromatography (hexane-ethyl acetate system) to provide the title compound (2.5 g).
WORKUP
后处理
- customThe title compound was synthesized
- temperaturethe solution was refluxed for 20 hours and 30 minutes
- temperaturethe solution was further refluxed for 22 hours 30 minutes
- filtrationthe solution was filtered through celite pad
- extractionextracted with ethyl acetate
- washwashed with brine
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- custompurified by silica gel column chromatography (hexane-ethyl acetate system)