新型三唑硫酮席夫碱的微波合成与结构表征  

Synthesis of Novel Triazole Thioketone Schiff-Bases Under Microwave Irradiation and Its Characterization

作　　者：陈野鹏[1] 吕仁刚[1] 宋良[1] 杨诏政[1] 

机构地区：[1]辽宁科技大学化学工程学院

出　　处：《光谱实验室》2013年第5期2483-2486,共4页Chinese Journal of Spectroscopy Laboratory

基　　金：辽宁省教育厅重点实验室基金项目(2008S127)

摘　　要：微波辐射条件下,以氨基均三唑硫醇与查尔酮为原料,通过亲核取代反应,制备了3-(4-氨基-5-巯基-3-对甲苯基均三唑-1-氮代)-1,3-二苯-1-丙酮(3),(3)与系列芳香醛经缩合反应,合成了4种三唑硫酮席夫碱(4a-4d)。探讨了各实验因素对收率的影响,得到了优化的工艺条件:n(芳香醛)∶n(氨基三唑硫酮)=1∶1.1微波功率500W,催化剂冰醋酸2mL,反应时间4—7min,溶剂DMF,收率为65%—77%。利用IR、M S、1H N M R对目标产物进行了结构表征。3-[4-Amino-3- （p-methylphenyl）-5-thioxo-4,5-dihydro-lH-1,2,4-triazol-l-yl]-l, 3- diphenylpropanal （3） was synthesized by nucleophilic substitution of 4-amino-3-phenyl -5-mercapto- 1, 2, 4-triazole and chalcone under microwave irradiation. The product then reacted with aryl aldehydes to give four novel triazolethione Schiff-base derivatives （4a-4d）. The influence of each experimental factor upon the product yield was discussed. The optimal process conditions were ascertained as follows, n （aromatic aldehyde） ： n （amino substituted triazolethione） = 1 ：1. 1, the amount of acetic acid was 2mL,the time 4--7min,microwave power 500W,the solvent DMF,and the yield were 65%--77%. The structures of the MS,1H NMR spectra. target compounds were characterized by means of IR,MS, 1H NMR spectra.

关 键 词：微波 三唑硫酮 席夫碱 表征 

分 类 号：O657.61[理学—分析化学]