反应详情

In a 150 mL round bottom flask was placed 6-phenylpyridazin-3-amine (2.5 g, 14.5 mmol), NaHCO3 (2.44 g, 29 mmol) and methanol (50 mL) then to this suspension was added Br2 (2.317 g, 14.5 mmol) drop wise over about 30 minutes at room temperature. The mixture was stirred for 16 h, then filtered and concentrated in vacuo. The residue was purified by chromatography (silica gel, 200-300 mesh, petroleum ether:ethyl acetate=2:1) to give 4-bromo-6-phenylpyridazin-3-amine (1.2 g, 33%) as a light orange solid. LC-MS: [M+H]+, 250.0, tR=1.487 min.

1. customIn a 150 mL round bottom flask was placed
2. filtrationfiltered
3. concentrationconcentrated in vacuo
4. customThe residue was purified by chromatography (silica gel, 200-300 mesh, petroleum ether:ethyl acetate=2:1)