HRID1607400

反应详情

EQUATION

反应方程式

HRID 1607400 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 17 hours
  3. customwhile removing water
  4. customformed during the reaction
  5. temperatureAfter cooling
  6. washthe reaction mixture was washed with a saturated sodium chloride aqueous solution
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was purified by silica gel flash column chromatography (eluent: benzene/hexane=1/1 by volume)