反应详情

To a solution of 4-bromo-2-[(3-ethoxy-3-oxopropanoyl)(propan-2-yl)amino]benzoic acid (6.2 g, 16.7 mmol) in 170 mL of DCE is added triethylamine (3.5 mL, 25.1 mmol), followed by addition of thionyl chloride (1.45 mL, 20.6 mmol) at 0° C. After stirring at room temperature for 3 hours, the reaction medium is diluted with DCM and washed with aqueous HCl solution (1M). The organic phase is washed with saturated aqueous NaHCO3 solution and saturated aqueous NaCl solution, dried over Na2SO4 and concentrated to dryness. The oil obtained is purified by flash chromatography (toluene/EtOAc: 100/0 to 90/10) to give 2,23 g of a white solid (yield: 52%).

1. washwashed with aqueous HCl solution (1M)
2. washThe organic phase is washed with saturated aqueous NaHCO3 solution and saturated aqueous NaCl solution
3. dry with materialdried over Na2SO4
4. concentrationconcentrated to dryness
5. customThe oil obtained
6. customis purified by flash chromatography (toluene/EtOAc: 100/0 to 90/10)