反应详情

温度

40 °C

A mixture of 2-(2,6-dichloro-4-trifluoromethylphenyl)-4,5-dicyanoimidazole (3.31 g, 0.01 mol) and sodium hydroxide (1.0 g, 0.025 mol) in water (10 ml) was stirred and heated at 40° C. overnight. Concentrated hydrochloric acid was added to the mixture and the precipitated solid was filtered off and purified by medium pressure liquid chromatography (mplc) on silica eluted with a mixture of ethyl acetate and dichloromethane (1:1). Recrystallization of the white solid from a mixture of ethyl acetate and petroleum spirit (bp 60°-80° C.) (1:1) gave 5-cyano-2-(2,6-dichloro-4-trifluoromethylphenyl)-imidazole-4-carboxamide (0.61 g), m.p. 254°-255° C., as a white solid.

1. filtrationthe precipitated solid was filtered off
2. custompurified by medium pressure liquid chromatography (mplc) on silica
3. washeluted with a mixture of ethyl acetate and dichloromethane (1:1)
4. customRecrystallization of the white solid
5. additionfrom a mixture of ethyl acetate and petroleum spirit (bp 60°-80° C.) (1:1)