Nitric Acid → HCID 69355199, compound

Participants

Reaction Steps

N-{2-Chloro-4-[(6,7-dimethoxy-4-quinolyl)oxy]phenyl}-N′-(5-methyl-3-isoxazolyl)urea (2.0 g) produced in Production Example was added to methanol (40 mL), 70% nitric acid (1.2 g) was added dropwise thereto, and the mixture was stirred at room temperature for 2 hr. The resultant precipitate was collected by filtration, and the filtered product was then dried under the reduced pressure. The resultant powder was stirred in N,N-dimethylformamide (10 mL) at 100° C. for complete dissolution of the powder. The solution was then cooled to room temperature, ethyl acetate (20 mL) was added dropwise thereto, and the mixture was stirred at that temperature overnight. The resultant precipitate was filtered, and the filtered product was then dried under the reduced pressure to give a form II crystal of N-{2-chloro-4-[(6,7-dimethoxy-4-quinolyl)oxy]phenyl}-N′-(5-methyl-3-isoxazolyl)urea nitrate (2.0 g, yield 91.0%).

Provenance & Evidence