HRID220065

反应详情

EQUATION

反应方程式

HRID 220065 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. customIn a test tube which had been dried
  2. temperatureby heating
  3. custompreheated to 100° C.
  4. extractionextracted 3× with methylene chloride
  5. washthe combined organic phases were washed with aqueous NaHCO3 solution
  6. dry with materialdried 20 over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure