微波辅助合成N-苯基哌嗪盐酸盐  

Synthesis of N-Phenylpiperazine Hydrochloride under Microwave Irradiation

作　　者：徐泽民[1,2] 李铭东 余卫国[4] 周文华[1,2] 

机构地区：[1]宁波市微循环与莨菪类药研究所 [2]宁波大学行为神经科学研究中心,浙江宁波315010 [3]宁波海曙优联生化研发有限公司,浙江宁波315010 [4]浙江医药高等专科学校,浙江宁波315100

出　　处：《化学世界》2012年第6期358-360,367,共4页Chemical World

基　　金：国家重点基础研究发展计划(973计划)(2009CB522008);宁波市科技计划项目(2009B21002)

摘　　要：在微波辅助下研究重要中间体N-苯基哌嗪盐酸盐合成的最佳条件。在微波辅助下苯胺与N,N-双(2-氯乙基)胺盐酸盐在溶剂乙二醇中经环合反应合成目标化合物。探讨了微波辐射时间、辐射温度、溶剂量、加入原料的摩尔比(苯胺∶N,N-双(2-氯乙基)胺盐酸盐)等因素对环化产率的影响。以最优化条件得到N-苯基哌嗪盐酸盐,最佳条件为:原料的摩尔比(苯胺∶N,N-双(2-氯乙基)胺盐酸盐)=1.0∶0.9,乙二醇的量与苯胺比为1mL∶5mmol,微波反应时间为15min,微波反应温度为120℃,收率84.34%。其结构经熔点、IR和1 H NMR和质谱与目标化合物的结构一致。该路线工艺流程简单、快速,三废少且易处理。The optimal synthetic conditions of the important intermediate compound N-phenyl piperazine hydrochloride were studied. Aniline and N, N-bis（2-chloroethyl）amine hydrochloride were reacted in the solvent of glycol under microwave. The factors affecting the ring formation reaction yield, such as reaction time, temperature, solvent amount and reaction substrates ratio were investigated. The opitimized conditions were as follow, aniline ： N, N-his （2-chloroethyl） amine hydro-chloride （mol ratio） = 1 ： 0. 9 ; glycol：aniline= 1 mL ： 5 mmol; reaction time 15 min; reaction temperature 120℃. The yield was 84.34%. The product was verified by IR ^1 H NMR and MS. The synthetic process is convenient, quick and less pollutaut.

关 键 词：苯胺 N-苯基哌嗪盐酸盐 微波辅助 

分 类 号：O624.6[理学—有机化学]