3,5-二碘苯磺酰氯的合成研究  

Synthesis of 3,5-Diiodobenzenesulfonyl Chloride

作　　者：郭理云 赵庆平 赵春深[1,2] 季春[1,2] 李焱[1,2,3] GUO Li-yun;ZHAO Qing-ping;ZHAO Chun-shen;JI Chun;LI Yan(School of Chemistry and Chemical Engineering;Guizhou Engineering Laboratory for Synthetic Drugs, School of Pharmacy;Research Institute of Advanced Technology, Guizhou University, Guiyang 550025, China)

机构地区：[1]贵州大学化学与化工学院,贵州贵阳550025 [2]贵州大学药学院贵州省合成药物工程实验室,贵州贵阳550025 [3]贵州大学先进技术研究院,贵州贵阳550025

出　　处：《化学试剂》2018年第4期389-392,共4页Chemical Reagents

基　　金：贵州省科技厅社发公关项目(黔科合SY字[2014]3054);贵州省科技合作计划项目(黔科合LH字[2015]7680,LH字[2016]7442号)

摘　　要：标题化合物是一种重要的化工中间体,广泛应用于医药、农药、材料等领域。目前,此化合物的合成路线未见文献报道。以4-硝基苯胺作为起始原料,经取代、重氮化、还原和磺化4步反应得到了标题化合物,探索了碘化剂、硫酸质量分数、还原剂、反应温度和亚硝酸投料量对产品收率的影响,优化了工艺条件,总收率达56.28%。其化学结构经IR、MS、~1HNMR和^（13）CNMR确证。该方法原料廉价易得、操作简单、反应条件较为温和且收率较高,适合工业化生产。3,5-Diiodobenzenesulfonyl chloride is an important chemical intermediates,and is widely used in medicine,pesticides,materials and other fields.The synthetic route is not reported in the literature.In this paper,the target compound was synthesized by substitution,diazotization,reduction,and sulfonation with 4-nitroaniline as the starting material.The effects of the iodination agent,sulfuric acid concentration,reducing agent,reaction temperature and nitrite dosage on the yield of the product were investigated,the technological condition had been optimized.The total yield was 56.28%.The chemical structure was confirmed by IR,MS,~1HNMR and^（13）CNMR.The raw materials are cheap and easy to get in this method.It is easy to operate and control and the yield was higher in each step.It is suitable for industrial production.

关 键 词：4-硝基苯胺 3 5-二碘苯磺酰氯 合成 

分 类 号：O626.1[理学—有机化学]