HRID247629

反应详情

EQUATION

反应方程式

HRID 247629 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

3.2 g of the 3-carboxethoxy-4-(2,3-dichlorophenyl)pyrrole obtained in (a) and 40 ml of a 1:1 mixture of methanol and 5N HCl are stirred for hours at 70° C. After it has cooled to room temperature, the reaction mixture is poured onto ice and extracted with ethyl acetate. The ester phase is in turn extracted with 10% sodium hydroxide solution. The aqueous extract is washed twice with ethyl acetate, acidified with hydrochloric acid and extracted with ethyl acetate. The organic phase is washed with water, dried over magnesium sulfate and filtered. The filtrate is concentrated by evaporation and the resultant 4-(2,3-dichlorphenyl)pyrrole-3-carboxylic acid melts at 180°-182° C.

WORKUP

后处理

  1. temperatureAfter it has cooled to room temperature
  2. additionthe reaction mixture is poured onto ice
  3. extractionextracted with ethyl acetate
  4. extractionextracted with 10% sodium hydroxide solution
  5. extractionThe aqueous extract
  6. washis washed twice with ethyl acetate
  7. extractionextracted with ethyl acetate
  8. washThe organic phase is washed with water
  9. dry with materialdried over magnesium sulfate
  10. filtrationfiltered
  11. concentrationThe filtrate is concentrated by evaporation