5-羧甲基环十五酮的合成工艺优化  

Synthetic Process Optimization of the 5-Ethyloic-cyclopentadecanone

作　　者：拾以萍[1] 郑苏[1] SHI Yiping;ZHENG Su(Jiangsu Provincial Xuzhou Pharmaceutical Vocational College,Xuzhou,Jiangsu 221116,China)

机构地区：[1]江苏省徐州医药高等职业学校,江苏徐州221116

出　　处：《化学世界》2018年第7期435-439,共5页Chemical World

基　　金：江苏省徐州医药高等职业学校课题(No.20150602)资助项目

摘　　要：以环十二酮和碳酸二甲酯为原料合成了5-羧甲基环十五酮,考察了和反应时间、催化剂的类型和用量、原料配比、原料投入方式、溴化物的种类等对中间体α-甲氧羰基环十二酮(1)2-溴丙烷-α-甲氧羰基环十二酮(2)收率的影响。结果表明,n(环十二酮)︰n(碳酸二甲酯)︰n(氢化钠)=1︰1.8︰2.7,碳酸二甲酯一次性加入,1,3-二溴丙烷为溴化剂,乙醇钠和六甲基膦酰三胺(HMPA)为催化剂,反应时间8h。此条件下,5-羧甲基环十五酮的收率为75%。5-Ethyloic-cyclopentadecanone was synthesized from cyclododecanone and dimethyl carbonate.The effects of reaction time,type and amount of catalyst,raw materials ratio,input method of raw materials and type of bromide on the yield ofα-methoxycarbonyl-cyclododecanone（1）and 2-bromopropane-α-methoxycarbonyl-cyclododecanone（2）were investigated.The results demonstrated that under the following optimized reaction conditions,which 1,3-dibromopropane was used as bromide,sodium ethoxide and hexamethyl phosphoryl triamide（HMPA）were used as catalysts,n（cyclododecanone）∶n（dimethyl carbonate）∶n（sodium hydride）=1∶1.8∶2.7,dimethyl carbonate was added at one time and the reaction time was 8 hours,the yield of 5-ethyloic-cyclopentadecanone could reach 75%.

关 键 词：中间体 环十五酮 5-羧甲基环十五酮 合成工艺优化 

分 类 号：TQ46[化学工程—制药化工]