反应详情

To solution of (4-bromo-2-chloro-phenoxy)-acetic acid (100 mg, 0.37 mmol), 2-amino isonicotinamide (77.89 mg, 0.56 mmol) and DMAP (92.58 mg, 0.75 mmol) in DMF 5 ml was added PyBOP (394.3 mg, 0.75 mmol), and stirred room temperature. Reaction mixture was poured onto ice cold water, diluted by methanol/MC mixture (10%). 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 PLC (EtoAC:Hexane:MeOH=3:6:1˜2:4:1) to afford 2-[2-(4-bromo-phenoxy)-acetylamino]-isonicotinamide as a colorless solid (0.076 g, 52% yield).

1. customReaction mixture
2. additionwas poured onto ice cold water
3. customThe organic phase was separated
4. washsequentially washed with aqueous sodium bicarbonate, brine and water
5. dry with materialdried over anhydrous MgSO4
6. concentrationconcentrated
7. customThe residue was purified by PLC (EtoAC:Hexane:MeOH=3:6:1˜2:4:1)