HRID5733
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
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
- temperaturethe mixture was refluxed for 2 hours
- additionThe reaction mixture was poured on ice
- extractionextracted twice with 1000 ml of chloroform
- washThe extract was washed with a saturated sodium chloride aqueous solution
- dry with materialdried over magnesium sulfate
- customevaporated
- customto remove the solvent under a reduced pressure
- customresulting residue
- washeluted with hexane/ethyl acetate (10:1)