反应详情

温度

60 °C

A mixture of 8.43 g of 4,5-dichloroimidazole, 80 ml of dimethylformamide and 1.83 g of sodium hydride is heated, with stirring, for 3 hours at 60° C. Subsequently, a solution of 23.04 g of 2-[(p-phenoxyphenoxy)-ethyl]p-toluenesulfonate in 40 ml of dimethylformamide is dripped in. The mixture is heated for 12 hours at 100° C., cooled, poured into 50 ml of ice water, and extracted several times with ethyl acetate, and the combined extracts are washed first with 5% strength aqueous sodium hydroxide solution and then with water. Drying over sodium sulfate, removal of the solvent under reduced pressure and recrystallization from methyl tert-butyl ether gives 16.9 g (81%) of N-[(p-phenoxyphenoxy)-ethyl]-4,5-dichloroimidazole; m.p.: 89°-91° C.

1. temperatureis heated
2. temperatureThe mixture is heated for 12 hours at 100° C.
3. temperaturecooled
4. extractionextracted several times with ethyl acetate
5. washthe combined extracts are washed first with 5% strength aqueous sodium hydroxide solution
6. dry with materialDrying over sodium sulfate, removal of the solvent under reduced pressure and recrystallization from methyl tert-butyl ether