HRID36556

反应详情

EQUATION

反应方程式

HRID 36556 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

16.9 g of diphenylamine, 50.0 g of 9,9-dimethylfluorene, 10.0 g of potassium carbonate anhydride and 3.0 g of copper powder were added to 70 ml of o-dichlorobenze, followed by stirring for 8 hours at 180°-185° C. After the reaction, the reaction mixture was cooled and subjected to filtration. The filtrate was concentrated under reduced pressure to obtain a solid. An appropriate amount of methylethylketone was added to the solid to obtain a crystal. The crystal was recovered by filtration and purified by silica gel column chromatography (eluent: toluene/hexane) to obtain 28.2 g of 2-(N,N-diphenyl)amino-9,9-dimethylfluorenone (Yield: 79%; melting point: 144.2°-145.1° C.).

WORKUP

后处理

  1. customAfter the reaction
  2. temperaturethe reaction mixture was cooled
  3. filtrationsubjected to filtration
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customto obtain a solid
  6. customto obtain a crystal
  7. filtrationThe crystal was recovered by filtration
  8. custompurified by silica gel column chromatography (eluent: toluene/hexane)