无溶剂下双氧水环氧化3-环己烯甲酸-3′-环己烯甲酯制备ERL-4221  

A Solvent-free Method for ERL-4221 by Epoxidation of 3-Cyclohexenylmethyl 3′-Cyclohexenecarboxylate with Hydrogen Peroxide

作　　者：章亚东[1] 储进昌[1] 王振兴[1] 马芳芳[1] 

机构地区：[1]郑州大学化工与能源学院,河南郑州450001

出　　处：《郑州大学学报（工学版）》2009年第4期58-61,共4页Journal of Zhengzhou University（Engineering Science）

基　　金：河南省自然科学基金资助项目(0511020800)

摘　　要：制备了氯甲基化聚苯乙烯-二乙烯苯接枝磷钨杂多酸季铵盐催化剂,用红外光谱和电感耦合等离子体原子发射光谱对催化剂进行了表征.无溶剂下以H2O2(w(H2O2)=34.5%)和3-环己烯甲酸-3′-环己烯甲酯(简称A)为原料,催化合成3,4-环氧基环己基甲酸-3′,4′-环氧基环己基甲酯(简称AOO),探讨了催化剂用量、n(A):n(H2O2)、反应时间、反应温度等因素对反应的影响.获得了适宜的合成条件为(以60mmol A计):反应温度65℃,反应时间100 min,催化剂用量5.0 g,n(A):n(H2O2)=1∶3.该条件下A的平均转化率达99%以上,AOO的平均产率达78.9%.催化剂平均回收率在93%以上.Chloromethylated polystyrene divinylbenzene grafted quaternary ammonium salt of phosphor-tungstic heteropoly acid had been prepared as a catalyst.The catalyst had been characterized by IR spectrum and inductively coupled plasma atomic emission spectrometry.3,4-Epoxycyclohexylmethyl-3′,4′-Epoxycyclohexane Carboxylate(AOO) had been synthesized by epoxidation of 3-Cyclohexenylmethyl 3′-Cyclohexenecarboxylate(A) with hydrogen peroxide(w(H 2O 2)=34.5%) as oxidant under organic solvent-free condition.The main inf...

关 键 词：无溶剂法 环氧化反应 3-环己烯甲酸-3′-环己烯甲酯 3 4-环氧基环己基甲酸-3 ′4′-环氧基环己基甲酯 

分 类 号：TQ235[化学工程—有机化工]