反应详情

温度

50 °C

At room temperature (about 20° C.), 4.9 g of 4-(6-chloro-2-pyridinyloxy)-phenol in 40 ml of anhydrous dimethylformamide is dripped into 0.6 g of 100% strength sodium hydride in 20 ml of anhydrous dimethylformamide. The mixture is subsequently stirred for 30 minutes at 50° C., and then 4.2 g of 1-chloromethyl-4,5-dichloroimidazole in 20 ml of anhydrous dimethylformamide is dripped in at room temperature. This mixture is stirred for 2 hours at 60° C. and overnight at room temperature. It is then stirred into 200 ml of ice water and the solution is extracted three times with methyl tert-butyl ether. The organic phase is washed with 5% strength sodium hydroxide solution and water, and dried, and the solvent is evaporated off under reduced pressure. The crude product obtained is recrystallized from toluene. There is obtained 6.6 g of 1-[4-(6-chloro-2-pyridinyloxy)-phenoxymethyl]-4,5-dichloroimidazole; m.p.: 94°-98° C.

1. customAt room temperature
2. customis dripped in at room temperature
3. stirringThis mixture is stirred for 2 hours at 60° C. and overnight at room temperature
4. extractionthe solution is extracted three times with methyl tert-butyl ether
5. washThe organic phase is washed with 5% strength sodium hydroxide solution and water
6. customdried
7. customthe solvent is evaporated off under reduced pressure
8. customThe crude product obtained
9. customis recrystallized from toluene