HRID1707289

反应详情

EQUATION

反应方程式

HRID 1707289 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

14.8g of aluminum chloride and 5g of veratrole are added to a solution of 7.34g of isophthalic acid monomethyl ester chloride in 160 ml of dichloromethane under ice cooling. The reaction mixture is refluxed for 8 hours, poured on ice water, acidified with 2 n of hydrochloric acid and shaken out with dichloromethane. The organic phase is dried on sodium sulfate, concentrated by evaporation and the residue is chromatographed on silica gel with hexane/ethyl acetate=8/2. 3.5g of 3-(4-hydroxy-3-methoxybenzoyl)-benzoic acid methyl ester of melting point of 133°-134° C. is obtained.

WORKUP

后处理

  1. temperatureThe reaction mixture is refluxed for 8 hours
  2. additionpoured on ice water
  3. customThe organic phase is dried on sodium sulfate
  4. concentrationconcentrated by evaporation
  5. customthe residue is chromatographed on silica gel with hexane/ethyl acetate=8/2