HRID1748491

反应详情

EQUATION

反应方程式

HRID 1748491 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Phosphoryl chloride (136.3 g) was slowly added dropwise to a solution of 1-(4-fluorophenyl)pyrrole (136.3 g) in N,N-dimethylformamide (250 ml) under ice cooling so as to keep the temperature of the reaction solution under 50° C., and then the mixture was stirred at room temperature for 24 hours. The reaction solution was made alkaline by pouring into an aqueous solution of potassium carbonate under ice cooling and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine and concentrated in vacuo. n-Hexane was added to the residue and the resulting precipitated solid was collected by filtration to give 1-(4-fluorophenyl)-2-formylpyrrole (152 g).

WORKUP

后处理

  1. customunder 50° C.
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with water and saturated brine
  4. concentrationconcentrated in vacuo
  5. additionn-Hexane was added to the residue
  6. customthe resulting precipitated solid
  7. filtrationwas collected by filtration