【摘要】 合成了重要的功能高分子中间体1,2-蒽乙二酮,最佳反应条件为:AlCl3在[Emim]Cl-AlCl3离子液体中的摩尔分数为0.67,离子液体与蒽的物质的量比为2,草酰氯与蒽物质的量比为2,反应温度为40℃,反应时间6h,1,2-蒽乙二酮产率可达91.5%,选择性达98.3%。且[Emim]Cl-AlCl3离子液体对环境污染小,并可循环使用。在相同实验条件下,对等物质的量的AlCl3、FeCl3、[Emim]Cl-AlCl3及[Emim]Cl-FeCl3的催化作用进行了对比,结果表明[Emim]Cl-AlCl3的效果最好。通过萃取、重结晶等方法得到了1,2-蒽乙二酮纯品,通过熔点测定、GC、GC/MS、FT-IR和1HNMR对反应产物进行定性和定量分析。更多还原

【Abstract】 [Bmim]Cl-AlCl3 ionic liquid was used as catalyst in the Friedel-Crafts acylation of anthracene with oxalyl chloride to synthesize the important macromolecular intermediate 1,2-aceanthrylenedione.The results showed that the suitable synthesis conditions of the acylation reaction were as follows:the molar ratio of AlCl3 in [Emim]Cl-AlCl3 ionic liquid was 0.67,the mass ratio of [Emim]Cl-AlCl3 versus anthracene was 2,the mass ratio of oxalyl chloride versus anthracene was 2,the reaction temperature was 40 ℃,and the reaction time was 6 h.Under these conditions,the yield of 1,2-aceanthrylenedione was 91.5% with the selectivity reaching 98.3%.Furthermore,[Emim]Cl-AlCl3 showed less pollution to the environment and could be recycled.Under the same reaction conditions,the effects of AlCl3,FeCl3,[Emim]Cl-AlCl3 and [Emim]Cl-FeCl3 at the same mol quantity on the yield and selectivity of 1,2-aeanthrylenedione were studied and the results indicated that [Emim]Cl-AlCl3 was the most effective catalyst.Pure 1,2-aceanthrylenedione was prepared by extraction and recrystallization and the structure of 1,2-aceanthrylenedione was identified by melting point measurement,GC/MS,FT-IR and 1HNMR analyses.更多还原