Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Beta-Alanine | HCID 239 | — |
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Reactant | HCID 68297595 | HCID 68297595 | — |
| Product | HCID 60151539 | HCID 60151539 | 48.8% |
Reaction Steps
A mixture of 1-benzyl-5-hydroxy-2-oxo-3-phenyl-1,2,3,4-tetrahydro-[1,7]naphthyridine-6-carboxylic acid methyl ester (22 mg, 0.057 mmol), β-alanine (657 mg, 7.4 mmol) and NaOMe solution (11 mL, 5.7 mmol, 0.5 M in MeOH) was refluxed for 48 h. After the mixture was cooled to r.t., the solvent was evaporated in vacuo. The residue was partitioned between EtOAc and water. 1 M HCl was added with vigorous stirring until pH about 2. The aqueous layer was extracted with additional EtOAc, and the organic layers were combined, dried over MgSO4, and concentrated. The residue was dissolved in saturated NaHCO3 and washed several times with ether. The aqueous layer was acidified to pH 2 with 4 M HCl, and the resulting precipitate was collected by filtration to give 12.4 mg of the title compound as a white solid. MS: (+) m/z 446.40 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09271970B2 |
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| Source dataset | uspto-grants-2016_03 |
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| ORD ID | ord-a57ce70201734c9f8426a304b35aa6c9 |
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| Source note | uspto-grants-2016_03 |
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