反应详情

To a solution of 6-(1-(6-bromo-[1,2,4]triazolo[4,3-a]pyridin-3-yl)ethyl)imidazo[1,2-b]pyridazin-2-amine TFA salt (250 mg, 0.52 mmol) in CH2Cl2 was added DIEA (0.65 g, 5.0 mmol) followed by cyclopropanecarbonyl chloride (0.16 g, 1.5 mmol). The reaction was stirred at ambient temperature for 30 min. Solvent was removed via rotary evaporation and the resulting residue was reconstituted in MeOH (10 mL). NH4OH (0.5 mL) was added and the reaction was stirred at ambient temperature for 1 hr. The reaction was then concentrated to dryness and the resulting material was dissolved in EtOAc, washed with saturated NaHCO3, dried with MgSO4, filtered and concentrated to dryness. The crude material was purified via MPLC (5% MeOH/0.1% NH4OH/EA) to provide the title compound, N-(6-(1-(6-bromo-[1,2,4]triazolo[4,3-a]pyridin-3-yl)ethyl)imidazo[1,2-b]pyridazin-2-yl)cyclopropanecarboxamide 48 (0.22 g, 0.52 mmol, 100%). 1H NMR (400 MHz, DMSO-d6) δ ppm 0.73-0.87 (m, 4 H) 1.83-1.99 (m, 4 H) 5.17 (d, J=7.07 Hz, 1 H) 7.38-7.57 (m, 3 H) 7.80 (d, J=9.60 Hz, 1 H) 7.99 (d, J=9.09 Hz, 1 H) 8.78 (s, 1 H) 11.14 (s, 1 H). ESI-MS:m/z 426.2 (M+H)+.

1. customSolvent was removed via rotary evaporation
2. additionNH4OH (0.5 mL) was added
3. stirringthe reaction was stirred at ambient temperature for 1 hr
4. concentrationThe reaction was then concentrated to dryness
5. dissolutionthe resulting material was dissolved in EtOAc
6. washwashed with saturated NaHCO3
7. dry with materialdried with MgSO4
8. filtrationfiltered
9. concentrationconcentrated to dryness
10. customThe crude material was purified via MPLC (5% MeOH/0.1% NH4OH/EA)