Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 67254666 | HCID 67254666 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 22046499 | HCID 22046499 | 64.9% |
Reaction Steps
To a stirred suspension of 5-methoxy-4-[3-(5-methyl-pyrazin-2-yl)-ureido]-2-trifluoromethyl-benzoic acid methyl ester (257 mg, 0.67 mmol) in 6.7 mL 3:1 MeOH:H2O at room temperature under nitrogen was added lithium hydroxide monohydrate (281 mg, 6.7 mmol) and the mixture was heated to 85° C. After stirring overnight the reaction was cooled to room temperature, MeOH was removed by rotovap and the residual suspension was neutralized with concentrated HCl to pH of approximately 5. The suspension was filtered and rinsed with H2O and the filter cake dried under high vacuum to give the acid as a white solid (161 mg, 61%). 1H-NMR (400 MHz, d6-DMSO) δ8.90 (br s, 1H), 8.63 (s, 1H), 8.22 (s, 1H), 7.38 (s, 1H), 4.00 (s, 3H), 2.42 (s, 3H). LRMS (esi, negative) m/e 369.0 (M−1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07067506B2 |
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| Source dataset | uspto-grants-2006_06 |
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| ORD ID | ord-e380ed42c81946468a9278b0b4cb512c |
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| Source note | uspto-grants-2006_06 |
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