Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 67254164 | HCID 67254164 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 22046272 | HCID 22046272 | 78% |
Reaction Steps
To a stirred suspension of 4-[3-(5-methyl-pyrazin-2-yl)-ureido]-3-trifluoromethoxy-benzoic acid methyl ester (136 mg, 0.37 mmol) in 4 mL 3:1 MeOH:H2O under nitrogen was added lithium hydroxide monohydrate (154 mg, 3.7 mmol), and the reaction heated to 65° C. The reaction turned yellow/green and eventually became a solution. After stirring overnight, the reaction was cooled to RT and partially concentrated by rotovap to remove most of the MeOH. The residual suspension was neutratized with 2N HCl until pH=6. The reaction formed a floculent precipitate which was filtered off with H2O and dried overnight under high vacuum to give the acid as a white solid (102 mg, 78%).
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-50fc5324ab8e4ad1b6a586195047a9dc |
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| Source note | uspto-grants-2006_06 |
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