HRID1670053

反应详情

EQUATION

反应方程式

HRID 1670053 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixed solution of 45 g of 1-bromopyrene, 21.7 g of 4-methylphenylboronic acid, 34 g of tribasic potassium phosphate, 10.3 g of tetrabutylammonium bromide, 0.71 g of palladium acetate, and 1.6 l (liters) of dimethylformamide was heated and stirred at 120° C. for 5 hours under a nitrogen stream. After the mixture was cooled to room temperature, 1.6 l of water was added thereto and stirred at room temperature for 0.5 hours. The precipitated solid was separated by filtration and washed twice with 200 ml of water. The resulting solid was dissolved in 500 ml of dichloromethane. The solution was dried over magnesium sulfate and then filtered through celite. The filtrate was evaporated, and the resulting residue was washed twice with 200 ml of methanol. The precipitated solid was separated by filtration and dried under vacuum to give 40 g of 1-(4-methylphenyl)pyrene.

WORKUP

后处理

  1. temperatureAfter the mixture was cooled to room temperature
  2. stirringstirred at room temperature for 0.5 hours
  3. customThe precipitated solid was separated by filtration
  4. washwashed twice with 200 ml of water
  5. dissolutionThe resulting solid was dissolved in 500 ml of dichloromethane
  6. dry with materialThe solution was dried over magnesium sulfate
  7. filtrationfiltered through celite
  8. customThe filtrate was evaporated
  9. washthe resulting residue was washed twice with 200 ml of methanol
  10. customThe precipitated solid was separated by filtration
  11. customdried under vacuum