HRID220065
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
- 90 °C
PROCEDURE
实验过程
In a test tube which had been dried by heating and preheated to 100° C., the degassed diluent mixture dioxane (2 ml)/water (0.7 ml) was added to N-(4-chloro-6-cyclopropylaminopyrimidin-5-yl)-2-ethylnicotinamide (0.41 mmol), sodium carbonate (3 eq) and 2,4-dichlorophenylboronic acid (2 eq). 5 mol % of tetrakis(triphenylphosphine)palladium(0) were added, and the reaction mixture was stirred at 90° C. for 3 hours. The mixture was then diluted with water and extracted 3× with methylene chloride, and the combined organic phases were washed with aqueous NaHCO3 solution, dried 20 over Na2SO4, filtered and concentrated under reduced pressure.
WORKUP
后处理
- customIn a test tube which had been dried
- temperatureby heating
- custompreheated to 100° C.
- extractionextracted 3× with methylene chloride
- washthe combined organic phases were washed with aqueous NaHCO3 solution
- dry with materialdried 20 over Na2SO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure