反应详情

温度

150 °C

A mixture of 7-benzyl-4-hydroxy-8-oxo-7,8-dihydro-[2,7]naphthyridine-3-carboxylic acid methyl ester (40 mg, 0.13 mmol), 3-Amino-2,2-dimethyl-propionic acid TFA salt (120 mg, 0.52 mmol) and NaOMe (56 mg, 1.03 mmol) in EtOH (2 mL) was heated at 150° C. for 6 h in a CEM microwave reactor. Solvent was evaporated in vacuo, and the residue was partitioned between water and EtOAc. 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 purified by silica gel chromatography (0-40% EtOAc/hexanes+2% AcOH) to give 32 mg of the title compound as a yellow solid. MS: (+) m/z 396.15 (M+1).

1. customSolvent was evaporated in vacuo
2. customthe residue was partitioned between water and EtOAc
3. addition1 M HCl was added
4. dry with materialThe organic layer was dried over MgSO4
5. concentrationconcentrated
6. customThe crude product was purified by silica gel chromatography (0-40% EtOAc/hexanes+2% AcOH)