HRID36556
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customAfter the reaction
- temperaturethe reaction mixture was cooled
- filtrationsubjected to filtration
- concentrationThe filtrate was concentrated under reduced pressure
- customto obtain a solid
- customto obtain a crystal
- filtrationThe crystal was recovered by filtration
- custompurified by silica gel column chromatography (eluent: toluene/hexane)