HRID1741040

反应详情

EQUATION

反应方程式

HRID 1741040 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-bromo-3-methylbenzonitrile (5 g, 0.026 mol) was suspended in 1,2-dimethoxyethane (100 ml) and treated with 4-boronobenzoic acid (2.4 g, 0.026 mol) followed by a solution of sodium carbonate (11.65 g, 0.11 mmol) in water (100 ml). The mixture was flushed with argon and tetrakis(triphenylphosphine)palladium (0) (0.55 g) was added. The reaction mixture was then heated to reflux with stirring. After 24 h, the 1,2-dimethoxyethane was removed by evaporation under reduced pressure and the aqueous residue was washed with ethyl acetate. The aqueous layer was then acidified to pH 1 and the resultant solid was filtered off and was dried in vacuo to give the title compound as a white solid (4.16 g, 69%).

WORKUP

后处理

  1. customThe mixture was flushed with argon and tetrakis(triphenylphosphine)palladium (0) (0.55 g)
  2. additionwas added
  3. temperatureThe reaction mixture was then heated
  4. temperatureto reflux
  5. customthe 1,2-dimethoxyethane was removed by evaporation under reduced pressure
  6. washthe aqueous residue was washed with ethyl acetate
  7. filtrationthe resultant solid was filtered off
  8. customwas dried in vacuo