p-Toluenesulfonic acid monohydrate → HCID 86630642, compound

Participants

Reaction Conditions

Reaction Steps

To N-[5-({2-[(cyclopropylcarbonyl)amino]imidazo[1,2-b]pyridazin-6-yl}oxy)-2-methylphenyl]-1,3-dimethyl-1H-pyrazole-5-carboxamide (2.00 g, 4.49 mmol) was added ethanol (80 mL), and the mixture was heated to 70° C. to give a uniform solution. p-Toluenesulfonic acid monohydrate (0.90 g, 4.71 mmol) was added to the mixture, and the mixture was naturally cooled to room temperature. 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 crystals were collected by filtration, and washed with hexane/ethanol (3:1). The obtained crystals were dissolved in ethanol (40 mL) by heating and the mixture was naturally cooled to room temperature. The precipitated crystals were collected by filtration and washed with ethanol. The crystals were dried at 70° C. for 3 hr under reduced pressure to give the title compound (2.34 g, 84%) as white crystals.

Provenance & Evidence