HRID1027313

反应详情

EQUATION

反应方程式

HRID 1027313 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

A mixed solution of 7.0 g of 1-bromopyrene, 4.7 g of 2-naphthaleneboronic acid, 11.6 g of tripotassium phosphate, 1.8 g of tetrabutylammonium bromide, 0.11 g of palladium acetate and 248 ml of dimethylformamide was heated with stirring under a nitrogen gas flow at 130° C. for 5 hours. After cooling the solution to room temperature, 300 ml of water was injected, followed by stirring at room temperature for 0.5 hours. The precipitated solid was collected by filtration and then washed twice with 100 ml of water. The resultant solid was dissolved in 200 ml of dichloromethane, dried over magnesium sulfate, evaporated and then filtered using Celite. The filtrate was evaporated and the residue was washed twice with 100 ml of methanol, and then the precipitated solid was collected by filtration. The solid was vacuum-dried to obtain 7.5 g of 1-(2-naphthyl)pyrene.

WORKUP

后处理

  1. temperatureAfter cooling the solution to room temperature
  2. stirringby stirring at room temperature for 0.5 hours
  3. filtrationThe precipitated solid was collected by filtration
  4. washwashed twice with 100 ml of water
  5. dissolutionThe resultant solid was dissolved in 200 ml of dichloromethane
  6. dry with materialdried over magnesium sulfate
  7. customevaporated
  8. filtrationfiltered
  9. customThe filtrate was evaporated
  10. washthe residue was washed twice with 100 ml of methanol
  11. filtrationthe precipitated solid was collected by filtration
  12. customThe solid was vacuum-dried