Water → 6-(6-(2,4-Difluorophenyl)-1-methyl-1H-imidazo[1,2-a]imidazol-5-yl)-3-isopropyl-[1,2,4]triazolo[4,3-b]pyridazine

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Reaction Steps

6-(2,4-Difluorophenyl)-5-(3-isopropyl-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)imidazo[2,1-b]oxazole (0.200 g, 0.526 mmol, Example #8), 40% methylamine in water (1.50 mL, 15.4 mmol) and 1,4-dioxane (1 mL) were heated in a CEM® microwave at about 120° C. (250 psi maximum pressure, 10 min ramp, 300 max watts) for about 55 min. The mixture was concentrated under reduced pressure then treated with HOAc (1.5 mL). The solution was stirred at ambient temperature for about 1 h then the material was purified by RP-HPLC (Table 1, Method f). The desired fractions were collected and concentrated under reduced pressure to remove most of the ACN. The precipitate which formed was collected by filtration and washed with water (3 mL) then dried overnight under vacuum at about 70° C. to give the title compound (0.115 g, 56%): LC/MS (Table 1, Method g) Rt=1.88 min; MS m/z: 394.2 (M+H)+.

Provenance & Evidence