反应详情

2-Bromo-3-fluorobenzoic acid (9.27 g), 1-N,O-dimethylhydroxylamine hydrochloride (4.129 g, 42.33 mmol), and PyBOP (22.03 g, 1 eq., 42.33 mmol) were suspended in DCM (400 mL). DIEA was then added and the resulting solution was stirred at room temp. for 14 h (no SM left by TLC). The solution was then washed with water, IN aq HCl and aq sat. NaHCO3 in succession. The organics were dried (MgSO4) and concentrated in vacuo. The residue was purified by ISCO (330 g SiO2, attached) to give 8.3 g (75%) of 2-bromo-3-fluoro-N-methoxy-N-methylbenzamide as a white solid. Rf˜0.5 (1:1 Hex:EtOAc); LC/MS ES+1: 261.99.

1. waitleft by TLC)
2. washThe solution was then washed with water, IN aq HCl
3. dry with materialThe organics were dried (MgSO4)
4. concentrationconcentrated in vacuo
5. customThe residue was purified by ISCO (330 g SiO2, attached)