HuagongsheHuagongshe Chemistry Print Report · For research reference only
Beta-Alanine → 3-[(3-Benzyl-5-hydroxy-2-oxo-1-phenyl-1,2-dihydro-[1,7]naphthyridine-6-carbonyl)-amino]-propionic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Beta-Alanine | HCID 239 | — |
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Reactant | 3-Benzyl-5-hydroxy-2-oxo-1-phenyl-1,2-dihydro-[1,7]naphthyridine-6-carboxylic acid methyl ester | HCID 68297447 | — |
| Product | 3-[(3-Benzyl-5-hydroxy-2-oxo-1-phenyl-1,2-dihydro-[1,7]naphthyridine-6-carbonyl)-amino]-propionic acid | HCID 68297409 | 45.1% |
Reaction Steps
A mixture of 3-benzyl-5-hydroxy-2-oxo-1-phenyl-1,2-dihydro-[1,7]naphthyridine-6-carboxylic acid methyl ester (25 mg, 0.065 mmol), β-alanine (767 mg, 8.6 mmol) and NaOMe solution (13 mL, 6.5 mmol, 0.5 M in MeOH) was refluxed for 16 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 was about 2. The organic layer was dried over MgSO4 and concentrated. The crude product was dissolved in saturated NaHCO3 and washed several times with ether. The aqueous layer was acidified to pH about 2, and the resulting precipitate was isolated by filtration to give 13 mg of the title compound. MS: (+) m/z 444.25 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09271970B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-1a02c3ad03704de5b5f4582b79caca1f |
| Source note | uspto-grants-2016_03 |