反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 85 °C
PROCEDURE
实验过程
To a mixture of tert-butyl 4-(5-((4-chloro-5-(trifluoromethyl)pyrimidin-2-yl)amino)pyridin-2-yl)piperidine-1-carboxylate A70 (0.208 g, 0.453 mmol), 1-(2-ethynylphenyl)cyclopropanecarboxamide K6 (0.079 g, 0.42 mmol), CuI (0.003 g, 0.02 mmol), PdCl2(PPh3)2 (0.017 g, 0.024 mmol) and t-Bu3PH.BF4 (0.009 g, 0.03 mmol) under a nitrogen atmosphere was added dioxane (6.0 mL) and DIPEA (0.23 mL, 1.3 mmol). The mixture was stirred at 85° C. for 4 hours and then concentrated under reduced pressure. Purification by silica gel column chromatography (Biotage Isolera, 0-100% EtOAc in Petroleum Benzine 40-60° C., 0-20% MeOH in EtOAc) gave the title compound A78 (0.118 g, 46%). LCMS-D: rt 3.645 min; m/z 607.4 [M+H]+.
WORKUP
后处理
- concentrationconcentrated under reduced pressure
- customPurification by silica gel column chromatography (Biotage Isolera, 0-100% EtOAc in Petroleum Benzine 40-60° C., 0-20% MeOH in EtOAc)