HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Methoxide → {2-[(7-Benzyl-1-cyano-4-hydroxy-8-oxo-7,8-dihydro-[2,7]naphthyridine-3-carbonyl)-amino]-ethoxy}-acetic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Reactant | 2-(2-aminoethoxy)acetic Acid | HCID 11170956 | — |
| Reactant | 7-Benzyl-1-cyano-4-hydroxy-8-oxo-7,8-dihydro-[2,7]naphthyridine-3-carboxylic acid methyl ester | HCID 68297608 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | {2-[(7-Benzyl-1-cyano-4-hydroxy-8-oxo-7,8-dihydro-[2,7]naphthyridine-3-carbonyl)-amino]-ethoxy}-acetic acid | HCID 68297143 | 12.6% |
Reaction Conditions
| Temperature | 150 °C |
|---|
Reaction Steps
A mixture of 7-benzyl-1-cyano-4-hydroxy-8-oxo-7,8-dihydro-[2,7]naphthyridine-3-carboxylic acid methyl ester (25 mg, 0.075 mmol), (2-amino-ethoxy)-acetic acid (60 mg, 0.50 mmol), and NaOMe (20 mg, 0.37 mmol) in EtOH (5 mL) was refluxed for 16 h, then heated at 150° C. in a microwave reactor for 2 h. Solvent was evaporated in vacuo, and the residue was partitioned between EtOAc and water. 1 M HCl was added with vigorous stilling until pH about 2, and the organic layer was dried over MgSO4 and concentrated. The crude product was purified by chromatography (5-80% EtOAc/hexanes+2% AcOH) to give 4 mg of the title compound as a pale yellow solid. MS: (+) m/z 423.19 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08921389B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-ca3ef8bc79c14aa4a548e5e6700c975e |
| Source note | uspto-grants-2014_12 |