反应详情

温度

120 °C

A mixture of 1-benzyl-8-hydroxy-5-iodo-2-oxo-1,2-dihydro-[1,6]naphthyridine-7-carboxylic acid methyl ester (86 mg, 0.197 mmol), tetramethyltin (0.14 mL, 0.99 mmol) and PdCl2(PPh3)2 (28 mg, 0.039 mmol) in DMF (4 mL) was heated at 120° C. for 2 h under N2 atmosphere. After cooling to r.t., EtOAc (50 mL) and brine (10 mL) were added. 1 M HCl was added until pH about 2-3. The aqueous layer was extracted with additional EtOAc, and the organic layers were combined, dried over MgSO4, and concentrated. The crude product was purified by silica gel chromatography (0-3% MeOH/CH2Cl2) to give 18 mg of the title compound as a white solid. MS: (+) m/z 325.28 (M+1).

1. temperatureAfter cooling to r.t.
2. extractionThe aqueous layer was extracted with additional EtOAc
3. dry with materialdried over MgSO4
4. concentrationconcentrated
5. customThe crude product was purified by silica gel chromatography (0-3% MeOH/CH2Cl2)