4-(咪唑-1-基)苯胺 → N-(4-(1H-imidazol-1-yl)phenyl)-4-methyl-2-phenyl-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepin-8-amine

HRID 10

反应方程式

HRID 10 反应方程式
CN1Cc2ccc(Cl)nc2OC(c2ccccc2)C1.Nc1ccc(-n2ccnc2)cc1>CC(=O)O.CC(=O)O.COCCOC.O=C([O-])[O-].[Cs+].[Cs+].[Pd].c1ccc(-c2ccccc2P(C2CCCCC2)C2CCCCC2)cc1>CN1Cc2ccc(Nc3ccc(-n4ccnc4)cc3)nc2OC(c2ccccc2)C1

参与物

7

反应条件

温度
100 °C

实验过程

[Reactants], 8-chloro-4-methyl-2-phenyl-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine (0.120 g, 0.44 mmol), Palladium(II) acetate (9.81 mg, 0.04 mmol), 2-(Dicyclohexylphosphino)biphenyl (0.015 g, 0.04 mmol) and Cesium carbonate (0.427 g, 1.31 mmol) in DME (2.5 mL) were placed in a microwave vial and flushed with argon. The reaction mixture was then run in the microwave at 100°C for 1 hr. Reaction not complete. Run for another 30 minutes in the microwave. Still not complete. Added 0.1 eq of Palladium(II)acetate and 0.1 eq of 2-(Dicyclohexylphosphino)biphenyl and let the reaction mixture run in the microwave for additional 45 minutes. Reaction complete. The reaction mixture was filtrated through celite and the filtrate was concentrated. The crude product was purified by preparative chromatography giving 0.072 g (41%) of the product. N-(4-(1H-imidazol-1-yl)phenyl)-4-methyl-2-phenyl-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepin-8-amine

来源与证据

ORD记录
ord-fa122fe6774f45c5b7a107c1460052d3
来源数据集
750 AstraZeneca ELN dataset
原始链接
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