反应详情

(2-Methanesulfonylamino-ethyl)-carbamic acid tert-butyl ester (77 mg, 0.32 mmol) was dissolved in CH2Cl2 (2 mL). Trifluoroacetic acid (1 mL) was added, and the mixture was stirred at r.t. for 2 h. Solvent and excess TFA were removed by evaporation, and the residue was taken up in EtOH (2 mL). NaOMe was added with vigorous stirring until pH about 8. The resulting cloudy solution was transferred to a microwave vial containing 7-benzyl-4-hydroxy-8-oxo-7,8-dihydro-[2,7]naphthyridine-3-carboxylic acid methyl ester (25 mg, 0.081 mmol), and the mixture was heated at 140° C. for 6 h in a microwave reactor. The mixture was diluted with EtOAc and washed with 0.1 M HCl. The organic layer was dried over MgSO4 and concentrated. The crude product was purified by silica gel chromatography (0-5% MeOH/CH2Cl2) to give 20 mg of the title compound as an off-white solid. MS: (+) m/z 417.30 (M+1).

1. customSolvent and excess TFA were removed by evaporation
2. additionNaOMe was added
3. stirringwith vigorous stirring until pH about 8
4. temperaturethe mixture was heated at 140° C. for 6 h in a microwave reactor
5. washwashed with 0.1 M HCl
6. dry with materialThe organic layer was dried over MgSO4
7. concentrationconcentrated
8. customThe crude product was purified by silica gel chromatography (0-5% MeOH/CH2Cl2)