反应方程式
COC(=O)c1cc(Cl)cc(B2OC(C)(C)C(C)(C)O2)c1.Nc1ccccc1>CC(C)(C)P(C(C)(C)C)C(C)(C)C.COCCOC.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=P([O-])([O-])[O-].[K+].[K+].[K+].[Pd].[Pd]>COC(=O)c1cc(Nc2ccccc2)cc(B2OC(C)(C)C(C)(C)O2)c1参与物
7
反应条件
- 温度
- 100 °C
实验过程
aniline (0.162 mL, 1.78 mmol) was added to methyl 3-chloro-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzoate (440mg, 1.48 mmol), TRIS(DIBENZYLIDENEACETONE)DIPALLADIUM(0) (13.59 mg, 0.01 mmol), tri- tert-butylphosphine (10.80 µL, 0.04 mmol) and potassium phosphate (441 mg, 2.08 mmol) in degassed DME (6 mL) at 20°C under nitrogen. The reaction was stirred at 100 °C for 2 days. The reaction mixture was diluted with Et2O (50 mL), and washed sequentially with water (50 mL) and saturated brine (50 mL). The organic layer was dried over MgSO4, filtered and evaporated. The crude product was purified by flash silica chromatography, elution 10 to 60% EtOAc in heptane.
来源与证据
- ORD记录
- ord-fbf696d6dcb34e7c9c731cbe586b831a
- 来源数据集
- 750 AstraZeneca ELN dataset
- 原始链接
- 查看来源
关联笔记
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