反应详情

To a mixture of 2-nitroimidazole 1 (17.7 mmol, 1 equiv.) and anhydrous potassium carbonate (70.74 mmol, 4 equiv.) in 20 mL of acetonitrile is added dropwise a solution of tert-butylbromoacetate (17.7 mmol, 1 equiv.) in 10 ml of acetonitrile. The mixture is stirred one night at room temperature and concentrated under vacuum. The residue is purified by chromatography on silica gel using a mixture CH2Cl2/MeOH 95/5 as eluent to give the expected compound as white powder in 71% yield. mp 95-97° C.; 1H NMR (DMSO-d6, 400 MHz) δ 1.46 (s, 9H), 4.99 (s, 2H), 7.06 (d, 1H, J=1.01 Hz), 7.17 (d, 1H, J=1.01 Hz). MS (ESI+/ESI−) m/z 226.15 [M−H]−, 262.13 [M+Cl]−, 250.20 [M+H]+

1. concentrationconcentrated under vacuum
2. customThe residue is purified by chromatography on silica gel using a mixture CH2Cl2/MeOH 95/5 as eluent