HRID1198103

反应详情

EQUATION

反应方程式

HRID 1198103 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-chloro-1-(chloromethyl)-2-(p-chlorophenyl)-5-(trifluoromethyl)pyrrole-3-carbonitrile (0.7 g, 0.002 mol) and dimethyldithiocarbamic acid, sodium salt (0.57 g, 0.004 mol) in dimethyl formamide is heated at 50°-55° for 30 minutes, cooled to room temperature and poured into water. The resultant mixture is extracted with ethyl acetate. The combined extracts are washed with a saturated sodium chloride give an orange oil residue. The residue is mixed with hot hexane, cooled and filtered to give an orange solid filtercake. Recrystallization of the solid from isopropanol gives the title product as a tan crystaline solid, 0.7 g (80% yield), mp 129°-131° C.

WORKUP

后处理

  1. temperatureis heated at 50°-55° for 30 minutes
  2. extractionThe resultant mixture is extracted with ethyl acetate
  3. washThe combined extracts are washed with a saturated sodium chloride
  4. customgive an orange oil residue
  5. temperaturecooled
  6. filtrationfiltered
  7. customto give an orange solid filtercake
  8. customRecrystallization of the solid from isopropanol