反应详情

温度

0 °C

3-(2-chloro-6-fluorophenyl)-5-(2-chloro-4-hydroxymethylphenyl)-1-methyl-1H-1,2,4-triazole (0.50 g) is dissolved in 1,2-dimethoxyethane (20 ml) and cooled to 0° C., to which is added sodium hydride (60%, 0.07 g) and the reaction mixture is stirred for 15 minutes. Then, a solution of 2,3-dichloro-5-trifluoromethyl pyridine (0.34 g) in 1,2-dimethoxyethane (10 ml) is added dropwise and stirred for 3 hours. On completion of the reaction, the reaction solution is warmed to room temperature and poured into water and extracted with ether. The organic layer is washed with water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The concentrate is purified by silica gel column chromatography to give 0.62 g of desired compound.

1. stirringstirred for 3 hours
2. customOn completion of the reaction
3. temperaturethe reaction solution is warmed to room temperature
4. extractionextracted with ether
5. washThe organic layer is washed with water
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated under reduced pressure
8. customThe concentrate is purified by silica gel column chromatography