HRID1852558

反应详情

EQUATION

反应方程式

HRID 1852558 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 18 g (50 mmol) of 1,6-dibromopyrene, 11 g (50 mmol) of N-phenylnaphthalen-2-amine, 0.16 g (0.7 mmol) of Pd(OAC)2, 0.5 g (1.4 mmole) of tri-tert-butylphosine, 6 g (75 mmol) sodium tert-butoxide was stirred in 200 ml dry toluene, the reaction mixture was then heat to 100° C. for about overnight under nitrogen. The solution was filtered. The toluene solution was removed under reduced pressure from the filtrate. The residue was extracted three times with dichloromethane and water, dried with MgSO4 and filtered, and the dichloromethane was removed under reduced pressure. The product was purified by column chromatography to get 9.2 g of product (yield 37%).

WORKUP

后处理

  1. filtrationThe solution was filtered
  2. customThe toluene solution was removed under reduced pressure from the filtrate
  3. extractionThe residue was extracted three times with dichloromethane and water
  4. dry with materialdried with MgSO4
  5. filtrationfiltered
  6. customthe dichloromethane was removed under reduced pressure
  7. customThe product was purified by column chromatography