反应详情

To a solution of 5-bromo-nicotinic acid (100 g, 0.5 mol) in THF (2 L) at 0° C., (COCl)2 (95 g, 0.74 mol) was added. After stirring for 0.5 h, Et3N (152 g, 1.5 mol) and O, N-dimethyl hydroxylamine. HCl (140 g, 1.5 mol) were added. The reaction mixture was stirred at room temperature for 2.5 hours and then water (200 mL) and EtOAc (500 mL) were added. The organic layer was separated, dried (MgSO4) and concentrated in vacuo to afford 5—the title compound as a brown oil in 82% yield, 100%.

1. stirringThe reaction mixture was stirred at room temperature for 2.5 hours
2. customThe organic layer was separated
3. dry with materialdried (MgSO4)
4. concentrationconcentrated in vacuo