HRID1865774

反应详情

EQUATION

反应方程式

HRID 1865774 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2.0 g of 1,3,5-tris(1-naphthylamino)benzene, 5.0 g of 4-iodobiphenyl, 3.7 g of potassium carbonate, 2 g of copper powder, 0.3 g of 18-crown-6 (or 1,4,7,10,13,16-hexaoxacyclooctadecane) and 10 mL of mesitylene (reaction solvent) were placed in a 100 mL capacity glass flask and the reaction was carried out at a temperature of 170° C. for 17 hours under a nitrogen atmosphere. After the reaction, the resultant reaction mixture was extracted with toluene and the toluene solution was subjected to silica gel chromatography to fractionate the reaction product. The reaction product was then purified by recrystallization from a mixed solvent of toluene/hexane and then by sublimation to provide 1.2 g of the desired 1,3,5-tris(N-(4-biphenylyl)-N-(1-naphthyl)amino)benzene (TBNAB). The yield was 32%.

WORKUP

后处理

  1. customAfter the reaction
  2. customthe resultant reaction mixture
  3. extractionwas extracted with toluene
  4. customThe reaction product was then purified by recrystallization from a mixed solvent of toluene/hexane