Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | Tivozanib | HCID 9911830 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 86603570 | HCID 86603570 | 80% |
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 (50 mL), methanesulfonic acid (1.3 g) was added dropwise thereto, and the mixture was stirred at room temperature for 4 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 ethanol (120 mL) under reflux for complete dissolution. 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 II crystal of N-{2-chloro-4-[(6,7-dimethoxy-4-quinolyl)oxy]phenyl}-N′-(5-methyl-3-isoxazolyl)urea methanesulfonate (1.9 g, yield 80.0%).
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-656c9ca3f35445f7af0910420e18135e |
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| Source note | uspto-grants-2007_01 |
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