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%.
作者
拾以萍
郑苏
SHI Yiping;ZHENG Su(Jiangsu Provincial Xuzhou Pharmaceutical Vocational College,Xuzhou,Jiangsu 221116,China)
出处
《化学世界》
CAS
CSCD
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
关键词
中间体
环十五酮
5-羧甲基环十五酮
合成工艺优化
intermediate
cyclopentadecanone
5-ethyloic-cyclopentadecanone
synthesis process optimization
