反应详情

温度

5 °C

To a solution of 800 mg of [2-(4-trifluoromethyl-phenyl)-4-(4-trifluoromethyl-piperidin-1-ylmethyl)-thiazol-5-yl]-methanol in 4 mL of tetrahydrofuran at 5° C. was slowly added 2.13 mL of a molar solution of potassium tert-butoxide in tert-butanol. After stirring at 5° C. for 30 minutes, the resulting solution was slowly added to a solution of 296 mg of 2,4,5-trifluoro-benzonitrile in 1 mL of tetrahydrofuran at −60° C. The resulting mixture was stirred for 1 h at −60° C. then stirred overnight allowing the temperature to warm up to room temperature. It was then poured into water and extracted with dichloromethane. The organic extracts were dried over magnesium sulfate, filtered and concentrated under reduced pressure. The crude product was recrystallized from methanol and washed with diisopropyl ether to give 890 mg of 2,5-difluoro-4-[2-(4-trifluoromethyl-phenyl)-4-(4-trifluoromethyl-piperidin-1-ylmethyl)-thiazol-5-ylmethoxy]-benzonitrile.

1. customat 5° C.
2. stirringThe resulting mixture was stirred for 1 h at −60° C.
3. stirringthen stirred overnight
4. temperatureto warm up to room temperature
5. extractionextracted with dichloromethane
6. dry with materialThe organic extracts were dried over magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. customThe crude product was recrystallized from methanol
10. washwashed with diisopropyl ether