反应详情

温度

55 °C

Ethyl 5-iodo-6-methyl-2-oxo-1-(3-trifluoromethylphenyl)-1,2-dihydro-pyridine-3-carboxylate (synthesised according to WO2005/026123, Example 63 (b)) (9.02 g, 20 mmol), 4-(5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazol-1-yl)benzonitrile (synthesised according to WO2009/061271, Example 1 intermediate) (8.85 g, 30.00 mmol), potassium hydrogenphosphate trihydrate (13.69 g, 60.00 mmol) and 1,1′-bis(di-tert-butylphosphino) ferrocene palladium dichloride (0.918 g, 1.40 mmol) were suspended in DMF (100 mL) in a 250 mL round-bottomed flask and the mixture was purged with argon. Then 1,1″-bis(di-tert-butylphosphino) ferrocene palladium dichloride (0.918 g, 1.40 mmol) was added and the reaction mixture was heated to 55° C. under vigorous stirring. After 30 and 90 min more 4-(5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazol-1-yl)benzonitrile (1.4 g, 4.74 mmol and 2.5 g, 8.47 mmol) was added.

1. customthe mixture was purged with argon