HRID1769281

反应详情

EQUATION

反应方程式

HRID 1769281 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1-amino-2-(2,6-dichloro-4-trifluoromethylbenzylideneamino)-1,2-dicyanoethylene (3.3 g, 0.01 mol) and 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (3.3 g, 0.01 mol) in acetonitrile (75 ml) was stirred at reflux for 48 hours. Evaporation of the solvent yielded a brown solid which was continuously extracted with boiling toluene. The solution was evaporated under reduced pressure and the red-brown residue was dissolved in a mixture of ethyl acetate and dichloromethane (1:10) and filtered through silica. Evaporation of the liltrate gave a brown solid which was triturated with hexane and the solid was removed by filtration to give 2-(2,6-dichloro-4-trifluoromethylphenyl)-4,5-dicyanoimidazole (1.4 g) as a light brown solid, m.p. 194°-195° C.

WORKUP

后处理

  1. temperatureat reflux for 48 hours
  2. customEvaporation of the solvent
  3. customyielded a brown solid which
  4. extractionwas continuously extracted with boiling toluene
  5. customThe solution was evaporated under reduced pressure
  6. dissolutionthe red-brown residue was dissolved in a mixture of ethyl acetate and dichloromethane (1:10)
  7. filtrationfiltered through silica
  8. customEvaporation of the
  9. customliltrate gave a brown solid which
  10. customwas triturated with hexane
  11. customthe solid was removed by filtration