HRID1275291

反应详情

EQUATION

反应方程式

HRID 1275291 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 30.8 g. p-toluoyl chloride and 26.6 g. (0.2 mole) of aluminum chloride in 250 ml. of 1,2-dichloroethane is added to a refluxing solution of 50.6 g. (0.2 mole) of ethyl 3-ethoxycarbonyl-1,4-dimethylpyrrole-2-acetate in 250 ml. of 1,2-dichloroethane over 30 minutes. The mixture is heated under reflux for 90 minutes, and poured into ice-diluted hydrochloric acid. The organic solution is separated, washed with brine, and dried over magnesium sulfate. The solvent is evaporated in vacuo, and the residue is recrystallized from methanol to give ethyl 1,4-dimethyl-3-ethoxycarbonyl-5-(p-toluoyl)-pyrrole-2-acetate as a white solid, m.p. 108-111° C.

WORKUP

后处理

  1. temperatureThe mixture is heated
  2. temperatureunder reflux for 90 minutes
  3. additionpoured into ice-diluted hydrochloric acid
  4. customThe organic solution is separated
  5. washwashed with brine
  6. dry with materialdried over magnesium sulfate
  7. customThe solvent is evaporated in vacuo
  8. customthe residue is recrystallized from methanol