SYNTHESIS OF FUNCTIONAL MACROMOLECULE INTERMEDIATE THROUGH COUPLING REACTION CATALYZED BY [bmim]Cl/F

来源 :Chinese Journal of Reactive Polymers | 被引量 : 0次 | 上传用户:information1005
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To obtain new functional aromatic polymer material, 3,3’-biacenaphthene, which is used as macromolecule intermediate of function aromatic polymer material, was synthesized through the coupling reaction of acenaphthene catalyzing by ionic liquid ([bmim]Cl/FeCl3) at mild reaction condition. Pure 3,3’-biacenaphthene was obtained by recrystalling and column chromatography from the reaction mixture and was determined by GC/MS, 1HNMR and FTIR analysis. The influence of various reaction conditions on the yield of 3,3’-biacenaphthene were studied by GC analysis. The result shows that the optimum synthesis conditions of the coupling reaction are as following: the molar ratio of FeCl3 to [Bmim]Cl being 3, the mole ratio of FeCl3 in [Bmim]Cl/FeCl3 to acenaphthene being 4, the reaction temperature being 20 ℃, the reaction time being 4h and the solvent of the reaction system being PhNO2. Under those conditions, the yield of the 3,3’-biacenaphthene will be 48.71 % and selectivity of that will be 78.56 %. Further more, [bmim]Cl/FeCl3 has no pollution to environments and can be reused. To obtain new functional aromatic polymer material, 3,3’-biacenaphthene, which is used as macromolecule intermediate of function aromatic polymer material, was synthesized through the coupling reaction of acenaphthene catalyzing by ionic liquid ([bmim] Cl / FeCl3) at mild reaction Pure 3,3’-biacenaphthene was obtained by recrystalling and column chromatography from the reaction mixture and was determined by GC / MS, 1H NMR and FTIR analysis. The influence of various reaction conditions on the yield of 3,3’-biacenaphthene were studied by GC analysis. The result shows that the optimum synthesis conditions of the coupling reaction are as follows: the molar ratio of FeCl3 to [Bmim] Cl being 3, the mole ratio of FeCl3 in [Bmim] Cl / FeCl3 to acenaphthene being 4 , the reaction temperature being 20 ℃, the reaction time being 4h and the solvent of the reaction system being PhNO2. Under those conditions, the yield of the 3,3’-biacenaphthene will be 48.71% and selectivity of that w ill be 78.56%. Further more, [bmim] Cl / FeCl3 has no pollution to environments and can be reused.
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