反应详情

温度

80 °C

DIPEA (48.2 mL, 276.86 mmol) was added to 6-chloro-3-(trifluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazine (24.65 g, 110.74 mmol) and 4-(piperidin-4-yl)phenol (20.61 g, 116.28 mmol) in DMF (200 mL). The resulting solution was stirred at 80° C. for 1 hour. The reaction mixture was cooled to room temperature, then evaporated to dryness and re-dissolved in DCM (1 L) and washed with water (2×1 L). The organic layer was washed with saturated brine (500 mL), then dried over MgSO4, filtered and evaporated to afford crude product. The crude product was triturated with ether to afford 4-[1-[3-(trifluoromethyl)[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]phenol (36.6 g, 91%) as a solid.

1. temperatureThe reaction mixture was cooled to room temperature
2. customevaporated to dryness
3. dissolutionre-dissolved in DCM (1 L)
4. washwashed with water (2×1 L)
5. washThe organic layer was washed with saturated brine (500 mL)
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. customevaporated
9. customto afford crude product
10. customThe crude product was triturated with ether