HRID2113630
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
- 115 °C
PROCEDURE
实验过程
In a sealed tube, dissolve 6-chloro-3′-trifluoromethyl-[2,2′]bipyridinyl-5-carbonitrile (242 mg, 0.853 mmol), CH3B(OH)2 (300 mg, 5.10 mmol), K2CO3 (1.6 g, 12 mmol), and Pd(PPh3)4 in a solution of dioxane (10 mL) and H2O (2 mL). Bubble argon through the mixture for 30 minutes and seal. Heat the mixture at 115° C. overnight. Cool the mixture to room temperature. Add H2O (20 mL) and extract with EtOAc (3×20 mL). Combine the organic extracts and wash with brine (60 mL). Dry the organic layer over Na2SO4 and remove the solvent under reduced pressure. Purify the crude product using silica gel chromatography eluting with EtOAc/hexane (1:1) to yield the title compound. MS 264.07 (M+1).
WORKUP
后处理
- customseal
- temperatureCool the mixture to room temperature
- extractionAdd H2O (20 mL) and extract with EtOAc (3×20 mL)
- washCombine the organic extracts and wash with brine (60 mL)
- dry with materialDry the organic layer over Na2SO4
- customremove the solvent under reduced pressure
- customPurify the crude product
- washeluting with EtOAc/hexane (1:1)