反应详情

温度

110 °C

A mixture of 6-chloro-N-(3-fluoropyridin-4-yl)-8-(isoxazol-3-ylamino)imidazo[1,2-b]pyridazine-3-carboxamide (20 mg, 0.054 mmol) and trans-cyclohexane-1,4-diamine (61.1 mg, 0.535 mmol) in NMP (0.4 mL) was heated at 110° C. overnight, then cooled to room temperature. The resulting mixture was purified by reversed-phase preparative HPLC. The desired fractions were concentrated and dried to give 18.7 mg of 6-((trans-4-aminocyclohexyl)amino)-N-(3-fluoro-4-pyridinyl)-8-(3-isoxazolylamino)imidazo[1,2-b]pyridazine-3-carboxamide as a beige solid. HPLC Rt=2.292 min (Chromolith SpeedROD 4.6×50 mm, 10-90% aqueous methanol containing 0.1% TFA, 4 min gradient, monitored at 220 nm), [M+1]=452.

1. temperaturecooled to room temperature
2. customThe resulting mixture was purified by reversed-phase preparative HPLC
3. concentrationThe desired fractions were concentrated
4. customdried