HRID864652

反应详情

EQUATION

反应方程式

HRID 864652 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-(p-chlorophenyl)-1-methyl-5-(trifluoromethyl)pyrrole-3-carbonitrile (5.0 g, 0.0176 mol) in carbon tetrachloride is treated with bromine (56 g, 0.0351 mol), heated at reflux temperature for 8 hours, cooled, washed sequentially with water, aqueous sodium metabisulfite and water, dried over sodium sulfate and concentrated in vacuo to give a solid residue. The residue is recrystallized from heptane to give the title produce as a white solid, 6.0 g (94% yield), mp 126°-129° C.

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux temperature for 8 hours
  3. temperaturecooled
  4. washwashed sequentially with water, aqueous sodium metabisulfite and water
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated in vacuo
  7. customto give a solid residue
  8. customThe residue is recrystallized from heptane
  9. customto give the title
  10. customproduce as a white solid, 6.0 g (94% yield), mp 126°-129° C.