反应详情

温度

80 °C

A 50 mL round-bottomed flask equipped with a condenser outfitted with a nitrogen inlet was charged with 6-((2,4-difluorophenyl)ethynyl)-3-isopropyl-[1,2,4]triazolo[4,3-b]pyridazine (0.500 g, 1.67 mmol, Preparation #J.1) in DMA (15 mL) to give a yellow solution. Sodium azide (0.327 g, 5.03 mmol) was added in one portion. The reaction mixture was heated at about 80° C. for about 16 h. The reaction mixture was partitioned between EtOAc and water. The layers were separated and the organic layer was washed with brine, dried over MgSO4, filtered, and concentrated in vacuo. One-half of the aqueous mixture was purified via RP-HPLC (Table 1, Method f) to provide the title compound after lyophilization (0.080 g, 14%): LC/MS (Table 1, Method b) Rt=1.8 min; MS m/z: 342.2 (M+H)+.

1. customA 50 mL round-bottomed flask equipped with a condenser
2. customoutfitted with a nitrogen inlet
3. customto give a yellow solution
4. customThe reaction mixture was partitioned between EtOAc and water
5. customThe layers were separated
6. washthe organic layer was washed with brine
7. dry with materialdried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated in vacuo
10. customOne-half of the aqueous mixture was purified via RP-HPLC (Table 1, Method f)