反应详情

温度

70 °C

To a suspension of 4,5-bis(bromomethyl)-3,6-dichloropyridazine (800 mg, 2.39 mmol) in 40 mL anhydrous THF was added with sodium carbonate (507 mg, 4.78 mmol) and tetrabutylammonium iodide (88.3 mg, 0.24 mmol). The reaction mixture was added with 4-methylbenzylamine (0.31 mL, 2.39 mmol) in 20 mL THF dropwisely for 2 h. The reaction mixture was heated at 70° C. for 8 h and concentrated. The crude material was dissolved in DCM and washed with water and brine. The organic solution was dried over Na2SO4 and concentrated to afford a crude oil. The mixture was purified by flash chromatography on silica gel, eluting with 10-80% EtOAc:heptane to afford a off-white solid (300 mg, yield: 41%).

1. concentrationconcentrated
2. dissolutionThe crude material was dissolved in DCM
3. washwashed with water and brine
4. dry with materialThe organic solution was dried over Na2SO4
5. concentrationconcentrated
6. customto afford a crude oil
7. customThe mixture was purified by flash chromatography on silica gel
8. washeluting with 10-80% EtOAc