反应详情

温度

100 °C

A mixture of methyl 4-(8-bromoimidazo[1,2-b]pyridazin-6-yl)benzoate (0.3 g, 0.904 mmol), 5,6-dimethoxypyridin-2-amine (0.167 g, 1.084 mmol), Pd2(dba)3 (52 mg, 0.09 mmol), BINAP (225 mg, 0.362 mmol) and Cs2CO3 (0.884 g, 2.712 mmol) in dioxane (20 mL) was heated to 100° C. for 16 h in a sealed tube under N2 atmosphere. The mixture was cooled and concentrated in vacuo. The residue was purified by chromatography (silica, 10 g, 200-300 mesh, ethyl acetate:petroleum ether=1:3) to afford methyl 4-(8-(5,6-dimethoxypyridin-2-ylamino)imidazo[1,2-b]pyridazin-6-yl)benzoate (0.518 g) as a yellow solid containing unidentified impurities. LC-MS: [M+H]+=406, tR=1.766 min.

1. temperatureThe mixture was cooled
2. concentrationconcentrated in vacuo
3. customThe residue was purified by chromatography (silica, 10 g, 200-300 mesh, ethyl acetate:petroleum ether=1:3)