HRID1607400
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
To a solution of 2.0 g of 3-benzoylpropionic acid methyl ester in 50 ml of dry benzene were added 0.7 ml of ethylene glycol and 0.01 g of anhydrous-p-toluene-sulfonic acid and the mixture was heated under reflux for 17 hours while removing water formed during the reaction by using a molecular sieve. After cooling, the reaction mixture was washed with a saturated sodium chloride aqueous solution, and concentrated under reduced pressure. The residue was purified by silica gel flash column chromatography (eluent: benzene/hexane=1/1 by volume) to obtain 1.8 g of 4,4-ethylenedioxy-4-phenylbutyric acid methyl ester.
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureunder reflux for 17 hours
- customwhile removing water
- customformed during the reaction
- temperatureAfter cooling
- washthe reaction mixture was washed with a saturated sodium chloride aqueous solution
- concentrationconcentrated under reduced pressure
- customThe residue was purified by silica gel flash column chromatography (eluent: benzene/hexane=1/1 by volume)