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-《郑州大学学报(工学版)》

文章信息/Info

Title:: A Solvent-free Method for ERL-4221 by Epoxidation of 3-Cyclohexenylmethyl3’-CyclOhexenecarboxylate with Hydrogen Peroxide

作者:: 章亚东; 储进昌; 王振兴; 等.; 郑州大学化工与能源学院,河南郑州,450001, 郑州大学化工与能源学院,河南郑州,450001, 郑州大学化工与能源学院,河南郑州,450001, 郑州大学化工与能源学院,河南郑州,450001

Author(s):: ZHANG Yadong; CHU Jinchang; WANG Zhenxing; etc; School of Chemical and Energy Engineering，Zhengzhou University，Zhengzhou 450001，China

Keywords:: solvent—free method; epoxidation; 3-Cyclohexenylmethyl一3 7-Cyclohexenecarboxylate; 3; 4-Epoxycyclohexylmethyl一3’; 4’-Epoxycyclohexane Carboxylate

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(H2

Abstract:: Chloromethylated polystyrene divinylbenzene grafted quaternary ammonium salt of phosphor—tungsticheteropoly acid had been prepared as acatalyst．The catalyst had been characterized by IR spectrum and inductively coupled plasma atomic emission spectrometry． 3，4-Epoxycyclohexylmethyl一3’，4’一EpoxycyclohexaneCarboxylate(A00)had been synthesized by epoxidation of 3一Cyelohexenylmethyl 3 7-Cyclohexeneearboxylate(A)with hydrogen peroxide(W(H202)=34．5％)as oxidant under organic solvent—free condition．The maininfluence factors in the reaction，such as mole ration of A to H2 02，reaction time，temperature，amounts ofcatalyst and SO on，had been studied．The appropriate reaction condition are as fallows(based on 60 mmolA)：reaction temperature 65℃，reaction time 100 minutes，catalyst 5．0 g，n(A)：n(H202)=1：3．Underthe condition．average conversion of A is more than 99％and average yield of AOO is 78．9％．The averagerecovery of catalyst is over 93％．