微波辅助合成噻萘普汀重要中间体三环酮  

Microwave assisted synthesis of the important intermediate tricyclic ketone of tianeptine

作　　者：吴春姗 汤军 郑兵 张桢桢 吴霖娇 WU Chun-shan;TANG Jun;ZHENG Bing;ZHANG Zhen-zhen;WU Lin-jiao(Department of Biological and Pharmaceutical Engineering,Wuhan Huaxia University of Technology,Wuhan 430223,China)

机构地区：[1]武汉华夏理工学院生物与制药工程院,湖北武汉430223

出　　处：《化学研究与应用》2017年第2期273-277,共5页Chemical Research and Application

基　　金：湖北省教育厅科学技术研究计划指导性项目(B2015368)资助;武汉理工大学华夏院科研基金项目(15005)资助

摘　　要：以4-氯-2-磺酰氯基苯甲酸甲酯为起始原料,在微波辅助的条件下进行缩合、水解、环合,合成得到噻萘普汀重要中间体三环酮,并采用均匀设计的方法对工艺进行优化。结果表明,在微波辅助的条件下缩合反应微波输出功率为800W,反应时间仅为8min;水解反应微波输出功率为800W,反应时间仅为20min;环合反应微波输出功率为80W,反应时间仅为10min;三步反应最高总收率达到78.38%。With4-chloro-2-sulfonyl chloride benzoic acid methyl ester as starting material,under the conditions of microwave assis-ted,the important intermediate namely tricyclic ketone was prepared through condensation,hydrolyzation,cyclization;and used uni-form design method to optimize the process.The results showed that the condensation reaction under the condition of microwave as-sisted microwave output power was800W,the reaction time was only8min;hydrolysis reaction of microwave output power was800W,the reaction time was only20min;cyclization reaction of microwave output power was80W,the reaction time was only10min;and three steps reaction highest total yield reached78.38%.

关 键 词：微波辅助 合成 三环酮 均匀设计 

分 类 号：O622.4[理学—有机化学]