反应详情

温度

120 °C

To a solution of 6-chloro-3-(2-(4-fluorophenyl)-2-methylpropylamino)pyridazine-4-carbonitrile (550 mg, 1.8 mmol, 1.0 equiv), 3-aminocarbonylphenylboronic acid, pinacol ester (330 mg, 2.0 mmol, 1.1 equiv) and aqueous K2CO3 (2.0 M, 5.0 mL, 5.4 mmol, 3.0 equiv) in dioxane (18 mL) was added Pd(dppf)Cl2 (150 mg, 0.18 mmol, 0.1 equiv). The mixture was stirred at 120° C. for 10 minutes in a microwave and allowed to cool to room temperature. The solvents were evaporated in vacuo, and the residue was dissolved in dichloromethane. The solution was filtered and the solvent dried over Na2SO4. Purification over silica gel using a gradient of 40-80% EtOAc/hexanes gave a yellow solid that was slurried with CH3CN to give the desired product (30 mg, 4.3%) as a yellow solid. m/z=390.2 [M+H]+.

1. temperatureto cool to room temperature
2. customThe solvents were evaporated in vacuo
3. dissolutionthe residue was dissolved in dichloromethane
4. filtrationThe solution was filtered
5. dry with materialthe solvent dried over Na2SO4
6. customPurification over silica gel using a gradient of 40-80% EtOAc/hexanes
7. customgave a yellow solid