HRID974212

反应详情

EQUATION

反应方程式

HRID 974212 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

331 g of Z-4,4'-Stilbene-dicarboxylic acid di-tert.-butyl ester in 1700 ml of absolute toluene are boiled under reflux for 3 hours together with 10.3 g of p-toluene sulphonic acid. The reaction mixture is then concentrated by evaporation and boiled under reflux for 4 hours with 104.2 g of NaOH, 1300 ml of H2O and 1300 ml of ethanol. The reaction mixture is filtered hot after the addition of active charcoal, diluted with about 3 l of H2O and extracted twice, in each case with 1 l of CH2Cl2. Concentrated HCl is then added to the aqueous phase. 230 g of Z-4,4'-stilbene dicarboxylic acid are obtained after suction filtration and drying.

WORKUP

后处理

  1. concentrationThe reaction mixture is then concentrated by evaporation
  2. temperatureunder reflux for 4 hours with 104.2 g of NaOH, 1300 ml of H2O and 1300 ml of ethanol
  3. filtrationThe reaction mixture is filtered hot
  4. additionafter the addition of active charcoal
  5. additiondiluted with about 3 l of H2O
  6. extractionextracted twice, in each case with 1 l of CH2Cl2
  7. additionConcentrated HCl is then added to the aqueous phase