HRID1090577

反应详情

EQUATION

反应方程式

HRID 1090577 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

25.9 g of p-chlorocinnamic acid was dissolved in 250 ml of methanol, to the solution was added 1.5 ml of concentrated sulfuric acid, and the mixture was refluxed for 2 hours. The reaction mixture was poured on ice, and the mixture was alkalized with sodium bicarbonate and extracted twice with 1000 ml of chloroform. The extract was washed with a saturated sodium chloride aqueous solution, dried over magnesium sulfate and evaporated to remove the solvent under a reduced pressure, and resulting residue was applied to a silica gel column and eluted with hexane/ethyl acetate (10:1), to obtain 26.5 g of the methyl p-chlorocinnamate.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 2 hours
  2. additionThe reaction mixture was poured on ice
  3. extractionextracted twice with 1000 ml of chloroform
  4. washThe extract was washed with a saturated sodium chloride aqueous solution
  5. dry with materialdried over magnesium sulfate
  6. customevaporated
  7. customto remove the solvent under a reduced pressure
  8. customresulting residue
  9. washeluted with hexane/ethyl acetate (10:1)