反応 #107
ord-8ce809cf74f44b02a581dcd94f0c1ae0
反応方程式
溶媒
反応条件
実験手順
1-(8-chloro-2-(pyridin-3-yl)-2,3-dihydropyrido[3,2-f][1,4]oxazepin-4(5H)-yl)ethanone (0.043 g, 0.14 mmol), Palladium(II) acetate (3.18 mg, 0.01 mmol), 2-(Dicyclohexylphosphino)biphenyl (4.96 mg, 0.01 mmol) and Cesium carbonate (0.138 g, 0.42 mmol) were placed in a microwave vial and flushed with argon. DME (2 mL) was added and the reaction mixture was run in the microwave at 100°C for 60 minutes. No product according to LCMS. Added 0.1 eq of Palladium(II) acetate (3.18 mg, 0.01 mmol) and 0.1 eq of 2-(Dicyclohexylphosphino)biphenyl (4.96 mg, 0.01 mmol) and flushed with argon. Run in the microwave at 100°C for 30 minutes and the reaction was complete. The reaction mixture was filtrated through celite and concentrated. The crude product was purified by prep-HPLC. The solvent was evaporated and partitioned between sat. NaHCO3 and dichloromethane. The organic layer was separated, dried (MgSO4) and concentrated giving 0.0234 g (35%) of the product.