반응 #371
ord-5b8b8e8b9f444b0ba792e38397226bc2
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실험 절차
3-methoxy-4-(4-methyl-1H-imidazol-1-yl)aniline (0.118 g, 0.49 mmol), Palladium(II) acetate (9.19 mg, 0.04 mmol), 2-(Dicyclohexylphosphino)biphenyl (0.014 g, 0.04 mmol) and Cesium carbonate (0.00 µmol) were put in a 5 mL microwave vial and sealed and purged with argon. (R)-2-chloro-6-(2-fluoroethyl)-8-phenyl-5,6,7,8-tetrahydropyrimido[5,4-f][1,4]oxazepine (0.126 g, 0.41 mmol) in DME (5 mL) was added. The reaction mixture was run in the microwave at 100°C for 60 minutes. Reaction still not complete. Additional palladium(II)acetate and 2-(dicyclohexylphosphino)biphenyl (small spatula) and the reaction was run again in the microwave for 60 minutes. The reaction mixture was filtrated through celite, concentrated and purified by preparative chromatography. The productcontaining fractions were pooled, concentrated and partitioned between sat. NaHCO3 (aq) and dichloromethane. The organic layer was washed with brine, dried (NaSO4) and concentrated giving (R)-6-(2-fluoroethyl)-N-(3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl)-8-phenyl-5,6,7,8-tetrahydropyrimido[5,4-f][1,4]oxazepin-2-amine (0.029 g, 14.93 %) as the product.