反应详情

温度

80 °C

To a reactor under inert atmosphere was added 73.84 g (0.38 mol) 3-chloro-6-(1-methyl-1H-pyrazol-4-yl)pyridazine, 90 g (0.38 mol) 2,2-difluoro-2-quinolin-6-ylacetohydrazide and 1200 mL 1-methoxy-2-propanol. Then 29.85 mL (0.455 mol) methane sulphonic acid was added and the reaction mixture was heated at 80° C. for 8 hours. After cooling to ambient temperature the mesylate salt of the title compound was filtered off from the reaction mixture. This salt was dissolved in a mixture of 400 mL ethanol and 300 mL water, after alkalisation at 80° C. with 50 mL ammonia (0.65 mol) in 200 mL water the free base of the title compound precipitates and was filtered off. This precipitate was dried at 50° C. and was subsequently re-crystallized from 2-propanol (1.8 L/mol) to yield the title compound in 75% yield.