反应详情

温度

80 °C

DIPEA (2.348 mL, 13.48 mmol) was added to 6-chloro-3-(trifluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazine (2 g, 8.99 mmol) and ethyl 4-(piperazin-1-yl)benzoate (2.316 g, 9.89 mmol, CAS 80518-57-6) in DMF (20 mL). The resulting solution was stirred at 80° C. for 2 hours. The reaction mixture was cooled to room temperature, then evaporated to dryness and redissolved in DCM (150 mL) and washed with water (100 mL). The organic layer was dried over MgSO4, filtered and evaporated to afford crude product which was triturated with ether. The solid was collected by filtration and dried under vacuum to give ethyl 4-[4-[3-(trifluoromethyl)[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperazin-1-yl]benzoate (3.40 g, 90%) as a solid.

1. temperatureThe reaction mixture was cooled to room temperature
2. customevaporated to dryness
3. dissolutionredissolved in DCM (150 mL)
4. washwashed with water (100 mL)
5. dry with materialThe organic layer was dried over MgSO4
6. filtrationfiltered
7. customevaporated
8. customto afford crude product which
9. customwas triturated with ether
10. filtrationThe solid was collected by filtration
11. customdried under vacuum