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作 者:李晓严 毛丽惠 LI Xiaoyan MAO Lihui(Department of Science and Technology, Xinyang University, Xinyang 464000, Chin)
出 处:《河南师范大学学报(自然科学版)》2016年第5期74-77,共4页Journal of Henan Normal University(Natural Science Edition)
基 金:河南省教育厅科学技术研究重点项目(14B150059);信阳师范学院华锐学院科研项目(2015yb34)
摘 要:以2,4,6-三氯苯酚、乙二酰氯为原料合成化学发光材料双(2,4,6-三氯苯基)乙二酸酯.讨论了以传统溶剂苯作为反应介质改变原料配比或添加催化剂等不同反应条件下的反应情况,并且与不同离子液体作为反应介质的反应情况作对比,结果表明:苯为反应介质时,乙二酰氯稍过量,不加催化剂是最优反应条件,利用最优条件以离子液体为反应介质进行反应,反应时间缩短了一半,比传统反应产率增加了40.8%,且后处理简单,利用回收的离子液体重复反应,产率不减少,实现离子液体重复利用,达到绿色合成之目的.Chemiluminescence material bis(2,4,6-trichorophenyl)oxalate was synthesized by using 2,4,6-trichlorophenols and oxalyl chloride as raw materials.The influences of the molar ratio,catalyst,as well as solvent type on the reaction were investigated,and the experimental results were screened out as follows:When the reaction was taken place in the traditionally organic solvent‘benzene',the optimum reaction condition could be simply reached by using a little excess of oxalyl chloride without any addition of ferric trichloride.When the solvent benzene was substituted by ionic liquids,it was found that the using of ionic liquids could halve the reaction time,enhance the reaction yield by 40.8%,as well as simplify the workup procedure of reaction.Moreover,the ionic liquid could be easily recovered and efficiently reused which realized the goal of green synthesis.
关 键 词:双(2 4 6-三氯苯基)乙二酸酯 2 4 6-三氯苯酚 1-丁基-3-甲基咪唑四氟硼酸盐 1-丁基-3-甲基咪唑六氟磷酸盐
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