1,3-环己二酮的高效缩合工艺研究  

Study on Efficient Condensation Process of 1,3-Cyclohexanedione

作　　者：赵磊[1] 吴雪珂 岳涛 Zhao Lei;Wu Xueke;Yue Tao(Organic Reaction in Aqueous Engineering Research Center of Shandong Province,Shandong Chemical Technology Academy of Qingdao University of Science&Technology,Jinan 250014,China)

机构地区：[1]青岛科技大学、山东化工研究院、山东省水相有机合成及高效清洁分离工程技术研究中心,山东济南250014

出　　处：《山东化工》2023年第23期4-6,共3页Shandong Chemical Industry

基　　金：泰山学者建设工程项目基金(编号ts20130918)。

摘　　要：使用缩合工艺由5-氧代己酸酯合成1,3-环己二酮。通过对比实验,确定缩合工艺最适宜的反应条件为:以5-氧代己酸甲酯为原料,甲醇钠为碱,N,N-二甲基乙酰胺为溶剂,采用高温加入5-氧代己酸甲酯的方式,于80℃反应5 min,1,3-环己二酮的收率为99%。该缩合工艺使用非质子高极性溶剂避免了聚合杂质的产生,使用高温加入原料的方式降低了水解杂质的产生,具有反应速度快、效率高、反应选择性好、收率高等优势。The synthesis of 1,3-cyclohexanedione from 5-oxohexanoate was carried out using a condensation process.Through comparative experiments,the optimum reaction conditions of the condensation process were determined as follows:methyl 5-oxohexanoate as the raw material,sodium methoxide as the base,and N,N-dimethylacetamide as the solvent,and the reaction was carried out by adding methyl 5-oxohexanoate at high temperature,at 85℃for 5 min,and the yield of 1,3-cyclohexanedione was 99%.The condensation process uses a nonprotonic highly polar solvent to avoid the production of polymeric impurities,and uses high temperature to add raw materials to reduce the production of hydrolytic impurities,which has the advantages of fast reaction speed,high efficiency,good reaction selectivity and high yield.

关 键 词：5-氧代己酸甲酯 甲醇钠 N N-二甲基乙酰胺 缩合 高温 高收率 

分 类 号：TQ234.2[化学工程—有机化工]