反应详情

温度

80 °C

To a solution of 4-(6-chloro-pyridazin-3-yl)-phenol (Step 2, 1 g, 4.84 mmol) and aniline (1.35 g, 14.52 mmol) in 20 mL of DMSO was added 5 drops of TFA. The reaction was heated to 80° C. for 16 h. The solution was cooled to RT and diluted with 100 mL of EtOAc. The organic phase was washed with 40 mL of water, 40 mL of brine, dried over Na2SO4 and concentrated in vacuo. The residue was purified by chromatography (50% EtOAc/hexane to EtOAc) to give the title compound as a white solid. MS (ESI pos. ion) m/z: 264.2(M+H). Calc'd Exact Mass for C16H13N3O: 263.29.

1. temperatureThe solution was cooled to RT
2. washThe organic phase was washed with 40 mL of water, 40 mL of brine
3. dry with materialdried over Na2SO4
4. concentrationconcentrated in vacuo
5. customThe residue was purified by chromatography (50% EtOAc/hexane to EtOAc)