HRID1045300

反应详情

EQUATION

反应方程式

HRID 1045300 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
78 °C

PROCEDURE

实验过程

Under an argon gas atmosphere, 128.0 g (1.049 mol) of phenylboronic acid, 300.0 g (1.163 mol) of 2,6-dibromonaphthalene, 24.2 g (21.0 mmol) of tetrakis(triphenylphosphine)palladium(0), 4.3 L of dimethoxyethane and 1.60 L of aqueous solution of 2M sodium carbonate were added together, and stirred at 78 degrees C. for 24 hours. The reaction mixture was added with toluene and water, and aqueous phase thereof was eliminated. After organic phase thereof was washed by water and dried with magnesium sulfate, the toluene was distilled away under reduced pressure. Residue thereof was refined by silica-gel column chromatography and recrystallized with hexane such that 108 g of 2-bromo-6-phenylnaphthalene was obtained at an yield of 36%.

WORKUP

后处理

  1. washAfter organic phase thereof was washed by water
  2. dry with materialdried with magnesium sulfate
  3. distillationthe toluene was distilled away under reduced pressure
  4. customrecrystallized with hexane such that 108 g of 2-bromo-6-phenylnaphthalene
  5. customwas obtained at an yield of 36%