反应详情

温度

100 °C

A mixture of 8-bromo-6-phenylimidazo[1,2-b]pyridazine (0.15 g, 0.55 mmol), 5,6-dimethoxypyridin-2-amine (0.092 g, 0.61 mmol), Pd2(dba)3 (32 mg, 0.055 mmol), BINAP (68 mg, 0.11 mmol) and Cs2CO3 (0.54 g, 1.65 mmol) in dioxane (20 mL) was heated to 100° C. for 16 h in a sealed tube under N2 atmosphere then concentrated and the residue purified by chromatography (silica gel, 10 g, 200˜300 mesh, ethyl acetate:petroleum ether=1:6) to afford N-(5,6-dimethoxypyridin-2-yl)-6-phenylimidazo[1,2-b]pyridazin-8-amine (49 mg, 26%) as a yellow solid. 1H NMR (300 MHz, CD3OD): δ 8.56 (s, 1H), 8.01-7.92 (m, 3H), 7.60 (s, 1H), 7.51-7.48 (m, 3H), 7.35 (d, 1H, J=8.4 Hz), 6.73 (d, 1H, J=8.4 Hz), 4.09 (s, 3H), 3.85 (s, 3H). LC-MS: [M+H]+, 348, tR=1.735 min, HPLC: 98.28% at 214 nm, 98.33% at 254 nm, tR=5.85 min.

1. concentrationthen concentrated
2. customthe residue purified by chromatography (silica gel, 10 g, 200˜300 mesh, ethyl acetate:petroleum ether=1:6)