反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureat reflux for 48 hours
- customEvaporation of the solvent
- customyielded a brown solid which
- extractionwas continuously extracted with boiling toluene
- customThe solution was evaporated under reduced pressure
- dissolutionthe red-brown residue was dissolved in a mixture of ethyl acetate and dichloromethane (1:10)
- filtrationfiltered through silica
- customEvaporation of the
- customliltrate gave a brown solid which
- customwas triturated with hexane
- customthe solid was removed by filtration