Water → HCID 21079510, Verbindung

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 acetonitrile (27 mL), a solution of p-toluenesulfonic acid monohydrate (2.5 g) in acetonitrile (27 mL) was added dropwise thereto, and the mixture was stirred at room temperature for 3 hr. The resultant precipitate was collected by filtration and the filtered product was then dried under the reduced pressure. The powder thus obtained was stirred in N,N-dimethylacetamide (10 mL) at 100° C. for complete dissolution. The solution was then cooled to room temperature, and water (10 mL) was added dropwise thereto. The mixture was cooled to 5° C. and 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 p-toluenesulfonate (2.3 g, yield 84.0%).

1. filtrationThe resultant precipitate was collected by filtration
2. customthe filtered product was then dried under the reduced pressure
3. customThe powder thus obtained
4. temperatureThe solution was then cooled to room temperature
5. temperatureThe mixture was cooled to 5° C.
6. stirringwas stirred at that temperature overnight
7. filtrationThe resultant precipitate was filtered
8. customthe filtered product was then dried under the reduced pressure

ORD-Eintrag

ord-8b6f8ff6236b47458fe3e3b3ecd6e21f

Quelldatensatz

uspto-grants-2007_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07166722B2