反应详情

温度

100 °C

To a mixture of 6-chloropyridazin-3-amine (5 g, 38.6 mmol), methyl 3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzoate (15.2 g, 58 mmol), Pd2(dba)3 (2.22 g, 3.86 mmol), X-phos (7.35 g, 15.44 mmol) and Na2CO3 (12.3 g, 115.8 mmol) in dioxane (150 mL) and water (15 mL) was heated to 100° C. with stirring for 6 h under N2. The solvent was removed in vacuo and the resulting residue was purified by chromatography (silica gel, 200-300 mesh, CH2Cl2:MeOH=20:1) to give methyl 3-(6-aminopyridazin-3-yl)benzoate (7.4 g, 84%) as a white solid. LC-MS: [M+H]+, 230.1, tR=1.111 min.

1. customThe solvent was removed in vacuo
2. customthe resulting residue was purified by chromatography (silica gel, 200-300 mesh, CH2Cl2:MeOH=20:1)