Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Nitric Acid | HCID 944 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Tivozanib | HCID 9911830 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 69355199 | HCID 69355199 | 88% |
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 powder thus obtained was stirred in methanol (200 mL) and water (100 mL) under reflux for complete dissolution of the powder. The solution was then 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 I crystal of N-{2-chloro-4-[(6,7-dimethoxy-4-quinolyl)oxy]phenyl}-N′-(5-methyl-3-isoxazolyl)urea nitrate (2.0 g, yield 88.0%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07166722B2 |
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| Source dataset | uspto-grants-2007_01 |
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| ORD ID | ord-85edfedaf1004aef917fdefdd38d561f |
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| Source note | uspto-grants-2007_01 |
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