Methanesulfonic Acid → N-[5-({2-[(cyclopropylcarbonyl)amino]imidazo[1,2-b]pyridazin-6-yl}oxy)-2-fluorophenyl]-1,3-dimethyl-1H-pyrazole-5-carboxamide methanesulfonate

참여 물질

반응 단계

A solution of N-[5-({2-[(cyclopropylcarbonyl)amino]imidazo[1,2-b]pyridazin-6-yl}oxy)-2-fluorophenyl]-1,3-dimethyl-1H-pyrazole-5-carboxamide (1.00 g, 2.23 mmol) in ethanol (50 ml) was stirred at 70° C. for 20 min. Methanesulfonic acid (0.17 mL, 2.33 mmol) was added to the mixture, and the mixture was further stirred for 10 min. The mixture was naturally cooled to room temperature, and the solvent was evaporated under reduced pressure. To the obtained residue was added hexane/ethanol (3:1, 40 mL), and the mixture was stirred at room temperature for 2 hr. The precipitated precipitate was collected by filtration, and washed with hexane/ethanol (3:1). The obtained precipitate was dissolved in ethanol (40 mL) by heating, and the mixture was naturally cooled to room temperature. The precipitated crystals were collected by filtration, ethyl acetate (20 mL) was added to the mixture, and the mixture was stirred at 80° C. by heating. After cooling the mixture to room temperature, the precipitate was collected by filtration, washed with ethyl acetate and dried under reduced pressure at 100° C. for 3 hr to give the title compound (0.32 g, 26%) as white crystals.

출처 및 근거