反应详情

温度

100 °C

Potassium carbonate (697 mg, 5.05 mmol) was added to a solution of 1,5-bis(4-methoxyphenyl)-1H-1,2,4-triazol-3-ol (0.3 g, 1.01 mmol) in dimethylformamide (3 mL). After 10 minute stirring, 2,2,2-trifluoroethyl iodide (0.497 mL, 5.05 mmol) was added to the mixture and the mixture was heated at 100° C. for 3 hours. After cooling, 100 mL of ethyl acetate and 20 mL of water were poured into the mixture. The organic layer was separated, washed with water and brine, and dried over magnesium sulfate. The solvent was removed under reduced pressure. The residue was purified by silica gel column chromatography (hexane-ethyl acetate 10:1-5:1). The desired product was triturated with hexane, isolated by filtartion, and dried in vacuo to give 1,5-bis(4-methoxyphenyl)-3-(2,2,2-trifluoroethoxy)-1H-1,2,4-triazole (205 mg, 53.6%).

1. temperatureAfter cooling
2. customThe organic layer was separated
3. washwashed with water and brine
4. dry with materialdried over magnesium sulfate
5. customThe solvent was removed under reduced pressure
6. customThe residue was purified by silica gel column chromatography (hexane-ethyl acetate 10:1-5:1)
7. customThe desired product was triturated with hexane
8. customisolated by filtartion
9. customdried in vacuo