HRID1029065

反应详情

EQUATION

反应方程式

HRID 1029065 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

40 parts of 9,9-dibutyl-2-iodofluorene, 3.7 parts of aniline, 30 parts of potassium carbonate, 6 parts of copper powders (200 meshes), and 0.87 parts of 18-crown-6 were dissolved in 50 parts of dimethylformamide (DMF), and the obtained solution was reacted in a nitrogen atmosphere at 160° C. for 24 hours. After completion of the reaction, the reaction product was filtrated, and the filtrate was then extracted with ethyl acetate-water. The ethyl acetate phase was dried over magnesium sulfate, and the ethyl acetate was then distilled away, thereby obtaining a brown tarry substance. This brown tarry substance was separated and purified by column chromatography (hexane-ethyl acetate) to obtain 15 parts of 9,9-dibutyl-N-(9,9-dibutylfluorenyl)-N-phenylfluorenamine (the following Compound (344)) in the form of a colorless crystal.

WORKUP

后处理

  1. customthe obtained solution was reacted in a nitrogen atmosphere at 160° C. for 24 hours
  2. customAfter completion of the reaction
  3. filtrationthe reaction product was filtrated
  4. extractionthe filtrate was then extracted with ethyl acetate-water
  5. dry with materialThe ethyl acetate phase was dried over magnesium sulfate
  6. distillationthe ethyl acetate was then distilled away
  7. customobtaining a brown tarry substance
  8. customThis brown tarry substance was separated
  9. custompurified by column chromatography (hexane-ethyl acetate)