反应详情

A mixture of 7-benzyl-4-hydroxy-8-oxo-7,8-dihydro-[2,7]naphthyridine-3-carboxylic acid methyl ester (150 mg, 0.48 mmol) and bis(2,4,6-trimethylpyridine)iodine(I) hexafluorophosphate (1.24 g, 2.42 mmol) in 5 mL of CH2Cl2 was stirred for 16 h at r.t. The mixture was diluted with 30 mL of CH2Cl2 and washed with 5% sodium thiosulfate and 1 M HCl. The organic layer was dried over MgSO4 and concentrated. The crude product was purified by silica gel chromatography (20-100% CH2Cl2/hexanes+2% AcOH) to give 136 mg of the title compound as an off-white solid. MS: (+) m/z 436.82 (M+1).

1. washwashed with 5% sodium thiosulfate and 1 M HCl
2. dry with materialThe organic layer was dried over MgSO4
3. concentrationconcentrated
4. customThe crude product was purified by silica gel chromatography (20-100% CH2Cl2/hexanes+2% AcOH)