HRID274738

反应详情

EQUATION

反应方程式

HRID 274738 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-(2,3-dichlorophenyl)pyrrole-3-carboxylic acid (2.43 g, 9.5 mmol) and triethylamine (7 mL, 50 mmol) in tetrahydrofuran is stirred for 15 minutes at room temperature and concentrated in vacuo to obtain a residue. A mixture of the residue, thionyl chloride (2.77 mL, 38 mmol) and N,N-dimethylformamide (0.73 mL, 9.5 mmol) is stirred overnight at room temperature and concentrated in vacuo to obtain a yellow oil. The oil is added to a concentrated ammonia solution and stirred for 1 hour. This mixture is filtered to give a solid. The solid is washed with water, dried and chromatographed using silica gel and a 4:1 hexanes/ethyl acetate mixture to obtain the title product as a white solid (1.6 g, mp 185°-190° C.).

WORKUP

后处理

  1. concentrationconcentrated in vacuo
  2. customto obtain a residue
  3. stirringis stirred overnight at room temperature
  4. concentrationconcentrated in vacuo
  5. customto obtain a yellow oil
  6. stirringstirred for 1 hour
  7. filtrationThis mixture is filtered
  8. customto give a solid
  9. washThe solid is washed with water
  10. customdried
  11. customchromatographed