HRID1755518

反应详情

EQUATION

反应方程式

HRID 1755518 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 4-diphenylaminophenyl boronic acid (1.25 g, 4.33 mmol), 2,5-dibromotoluene (2.16 g, 8.65 mmol), Pd(PPh3)4 (0.25 g, 0.22 mmol) and K2CO3 (1.38 g, 10 mmol) in dioxane/water (50 mL/9 mL) was degassed and heated at 80° C. for 15 hours. The resulting mixture was mixed with ethyl acetate/brine. The organic phase was dried over Na2SO4, loaded on silica gel, and purified by flash column (hexanes to hexanes/dichloromethane 9:1 to 4:1). The desired fraction was collected and concentrated. After removal of solvent, a white solid (Compound 18) was obtained (1.2 g, in 67% yield).

WORKUP

后处理

  1. customwas degassed
  2. additionThe resulting mixture was mixed with ethyl acetate/brine
  3. dry with materialThe organic phase was dried over Na2SO4
  4. custompurified by flash column (hexanes to hexanes/dichloromethane 9:1 to 4:1)
  5. customThe desired fraction was collected
  6. concentrationconcentrated
  7. customAfter removal of solvent