反应详情

温度

0 °C

To a suspension of (3S,4S)-benzyl 3-((2-bromo-7-carbamoylimidazo[1,2-b]pyridazin-8-yl)amino)-4-(fluoromethyl)pyrrolidine-1-carboxylate (240 mg, 0.488 mmol) in acetonitrile (3 ml) at 0° C. was added iodotrimethylsilane (0.266 ml, 1.954 mmol) dropwise. The reaction mixture was stirred at 0° C. for 10 min and at room temperature for 1.5 h. The reaction was cooled to 0° C. and quenched with MeOH (2 ml). The resulting suspension was stirred at 0° C. for 30 min, filtered, washed with ethyl ether, and dried under vacuum to afford 2-bromo-8-(((3S,4S)-4-(fluoromethyl)pyrrolidin-3-yl)amino)imidazo[1,2-b]pyridazine-7-carboxamide, hydroiodide as an off-white solid. ESI-MS (analytical LCMS Method A): m/z 357.0 ([M+H]+).

1. temperatureThe reaction was cooled to 0° C.
2. customquenched with MeOH (2 ml)
3. stirringThe resulting suspension was stirred at 0° C. for 30 min
4. filtrationfiltered
5. washwashed with ethyl ether
6. customdried under vacuum