反应详情

A mixture of 7-(2,4-dimethoxy-benzyl)-4-hydroxy-8-oxo-7,8-dihydro-[2,7]naphthyridine-3-carboxylic acid methyl ester (25 mg, 0.068 mmol), glycine (675 mg, 8.9 mmol) and NaOMe solution (13.5 mL, 6.8 mmol, 0.5 M in MeOH) was refluxed for 16 h. Solvent was evaporated in vacuo, and the residue was dissolved in saturated NaHCO3 and washed with ether. The aqueous layer was acidified with 4 M HCl to pH about 1, and the resulting precipitate was isolated by filtration. The crude solid was further purified by silica gel chromatography (10-90% EtOAc/hexanes+2% AcOH) to give 12 mg of the title compound as a light yellow solid. MS: (+) m/z 414.31 (M+1).

1. temperaturewas refluxed for 16 h
2. customSolvent was evaporated in vacuo
3. dissolutionthe residue was dissolved in saturated NaHCO3
4. washwashed with ether
5. customthe resulting precipitate was isolated by filtration
6. customThe crude solid was further purified by silica gel chromatography (10-90% EtOAc/hexanes+2% AcOH)