HRID1090743

反应详情

EQUATION

反应方程式

HRID 1090743 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
30 °C

PROCEDURE

实验过程

Methyl 4-tridecanoylpyrrole-2-carboxylate dithioethylene ketal (15.06 g, 37.9 mmol) prepared in Synthetic Example 8 was added to a mixed solution of 750 ml of ethanol and 150 ml of Raney-nickel (activated type, manufactured by Aldrich Co.) which was washed with water and ethanol successively. The mixture was heated under reflux for 30 minutes. After cooling it to ca. 30° C., the Raney-nickel was filtered off and the filtrate was concentrated under reduced pressure. Recrystallization of the residue from ethanol gave 10.70 g (91.8% yield) of methyl 4-tridecylpyrrole-2-carboxylate as white crystals, m.p. 80°-82° C.

WORKUP

后处理

  1. washwas washed with water and ethanol successively
  2. temperatureThe mixture was heated
  3. temperatureunder reflux for 30 minutes
  4. filtrationthe Raney-nickel was filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customRecrystallization of the residue from ethanol