文献类型：期刊文献

中文题名：TOSPA复合物的制备及其结构表征

英文题名：Preparation and characterization of TOSPA complex

作者：吴福忠[1];龙中柱[2];张平[1];蔡水洪[2];赵洪亮[1]

机构：[1]华东理工大学化工学院,上海200237;[2]上海东岳生物化工有限公司,上海200237

年份：2010

卷号：61

期号：10

起止页码：2731

中文期刊名：化工学报

外文期刊名：CIESC Journal

收录：CSTPCD;;EI(收录号：20104613383615);Scopus;北大核心:【北大核心2008】；CSCD:【CSCD2011_2012】；

语种：中文

中文关键词：TOSPA;TEBA;氯代反应;复合物;单晶

外文关键词：TOSPA; TEBA; chlorination; complex; single crystal

摘要：4,1′,6′-三氯-2,3,6,3′,4′-五乙酰基蔗糖(TOSPA)是全基团法制备三氯蔗糖的关键中间体,采用苄基三乙基氯化胺(TEBA)为催化剂,氯化亚砜为氯化剂合成了TOSPA。研究结果表明:氯化亚砜用量、反应温度对收率有较大影响,当氯化亚砜过量50%,90℃下反应6h,收率达到90%。实验中制备了TOSPA与甲苯的复合物,并经X射线单晶衍射、核磁、红外、元素分析进行了验证。利用TOSPA与甲苯复合物的物理特性,分离纯化得到了高纯度的TOSPA,具有工业化应用的前景。
4,1′,6′-Trichloro-2,3,6,3′,4′-sucrose pentaacetate（TOSPA）,as the key intermediate of sucralose,was synthesized by chlorination which treated with thionyl chloride and catalyst TEBA.The yield was up to 90% by applying the optimized conditions [SOCl2 150% （mol）,toluene,90℃,6 h]which was explored by the two important factors including amount of thionyl chloride and reaction temperature.The TOSPA complex was formed by mono-TOSPA and mono-toluene which was characterized by X-ray,1H NMR,IR and EA.The TOSPA with high purity was obtained by separation utilizing the complex physical characteristic.The process is of potential for industrial application.