反应详情

To solution of (4-bromo-2-chloro-phenoxyacetic acid (100 mg, 0.378 mmol), 2-amino isonicotinic acid methyl ester (86.42 mg, 0.568 mmol) and DMAP (69.43 mg, 0.568 mmol) in DMF 2 mL was added PyBOP (295 mg, 0.568 mmol) at room temperature. Reaction mixture was stirred at room temperature. Resulting mixture poured onto ice cold water, was diluted by ethyl acetate. The organic phase was separated, sequentially washed with aqueous sodium bicarbonate, brine and water, dried over anhydrous MgSO4, and concentrated. The residue was purified by flash silica gel column chromatography (EtoAC:Hexane=1:9˜4:6) to give 2-[2-(4-bromo-2-chloro-phenoxy)-acetylamino]-isonicotinic acid methyl ester as a colorless solid (0.084 g, 56% yield).

1. customReaction mixture
2. customResulting mixture
3. additionpoured onto ice cold water
4. customThe organic phase was separated
5. washsequentially washed with aqueous sodium bicarbonate, brine and water
6. dry with materialdried over anhydrous MgSO4
7. concentrationconcentrated
8. customThe residue was purified by flash silica gel column chromatography (EtoAC:Hexane=1:9˜4:6)