反应详情

温度

80 °C

48% HBr (13 ml) was added to (4-methoxy-benzyl)-[1,5]naphthyridin-4-yl-amine 485 (0.5 g, 1.88 mmol) and the mixture was heated at 80° C. for 2 h. After cooling, the mixture was neutralized with sat. NaHCO3 solution and the aqueous phase was extracted with EtOAc (80 ml). The organic phase was washed with water, dried (Na2SO4) and concentrated in vacuo. The crude residue was purified by column chromatography with DCM/MeOH/Aq. NH3 (97:2:1) as the eluent to give the title compound (0.25 g, 90%).

1. temperatureAfter cooling
2. extractionthe aqueous phase was extracted with EtOAc (80 ml)
3. washThe organic phase was washed with water
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated in vacuo
6. customThe crude residue was purified by column chromatography with DCM/MeOH/Aq