反应详情

温度

100 °C

8-chloro-4-methyl-2-(2,2,2-trifluoroethyl)-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine (60 % purity, 314 mg, 0.67 mmol), 6-methoxy-5-(1-methyl-1H-pyrazol-4-yl)pyridin-2-amine (137 mg, 0.67 mmol), PALLADIUM(II) ACETATE (15.07 mg, 0.07 mmol), 2-(DICYCLOHEXYLPHOSPHINO)BIPHENYL (23.53 mg, 0.07 mmol) and Cs2CO3 (328 mg, 1.01 mmol) were placed in a microwave vial. The vial was capped and flushed with argon. DME (3 mL) was added via a syringe and the resulting mixture was heated to 100°C in a microwave apparatus for 2 h. The reaction mixture was diluted with dichloromethane, filtered and concentrated. The residue was purified first by column chromatography using Silica stationary phase and gradient elution with increasing concentration of methanol, from 0 to 8 %, in dichloromethane, and then by reversed phase HPLC to give N-(6-methoxy-5-(1-methyl-1H-pyrazol-4-yl)pyridin-2-yl)-4-methyl-2-(2,2,2-trifluoroethyl)-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepin-8-amine (102 mg, 33.9 %).