反应详情

Hunig's base [7087-99-5] (1.8 mL, 10.3 mmol) was added to an ambient temperature stirred suspension of 3-bromo-6-piperazin-1-yl-imidazo[1,2-b]pyridazine dihydrochloride (907.1 mg, 2.6 mmol) in ethyl acetate (50 mL). After 30 minutes, pivaloyl chloride [3282-30-2] (0.3 mL, 2.5 mmol) was added and the suspension stirred under N2 blanket for 17 h then washed with brine, dried (MgSO4), and diluted with heptane. Chilling the stirred solution crystallized out a white powder which was isolated by filtration, 618.5 mg. LRMS (ESI) m/z 366.0/368.0 [(M+H)]+, calc'd for C16H20BrN6O: 366.26.

1. stirringthe suspension stirred under N2 blanket for 17 h
2. washthen washed with brine
3. dry with materialdried (MgSO4)
4. additiondiluted with heptane
5. temperatureChilling the stirred solution
6. customcrystallized out a white powder which
7. customwas isolated by filtration, 618.5 mg