Reacción #2484251

Ecuación de reacción

3,3',4,4'-tetramethyldiphenylamine

4-iodobiphenyl

potassium carbonate

→

N,N-bis(3,4-dimethylphenyl)biphenyl-4-amine

Rendimiento 71.2%

Disolventes

n-tridecane

Condiciones de reacción

Tratamiento posterior

1. 1
   OtroIn a 500-ml three-neck flask were placed
2. 2
   Otrothe reaction for 28 hours at 200° C. under a nitrogen gas stream
3. 3
   OtroThe reaction mixture was subjected to a column purification (solvent: n-hexane/toluene =10/1) with activated alumina
4. 4
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure
5. 5
   OtroThe residue was recrystallized from a mixed solvent of ethyl acetate and ethanol

Procedimiento

In a 500-ml three-neck flask were placed 31 g of 3,3',4,4'-tetramethyldiphenylamine synthesized in Example 3 (1), 40 g of 4-iodobiphenyl, 19 g of anhydrous potassium carbonate, 2 g of copper sulfate pentahydrate and 20 ml of n-tridecane, and after carrying out the reaction for 28 hours at 200° C. under a nitrogen gas stream, the reaction mixture was cooled to room temperature. The reaction mixture was subjected to a column purification (solvent: n-hexane/toluene =10/1) with activated alumina and the solvent was distilled off under reduced pressure. The residue was recrystallized from a mixed solvent of ethyl acetate and ethanol to provide 37 g of N,N-bis(3,4-dimethylphenyl)biphenyl-4-amine. (Melting point 119° to 120.5° C., colorless crystals, IR spectrum shown in FIG. 4)

Fuente