CIESC Journal ›› 2010, Vol. 61 ›› Issue (10): 2731-2737.
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WU Fuzhong; LONG Zhongzhu;ZHANG Ping; CAI Shuihong; ZHAO Hongliang
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吴福忠;龙中柱;张平;蔡水洪;赵洪亮
Abstract:
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,H 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.
Key words: TOSPA, TEBA, 氯代反应, 复合物, 单晶
TOSPA,
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6 h,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。
关键词: TOSPA, TEBA, 氯代反应, 复合物, 单晶
WU Fuzhong, LONG Zhongzhu, ZHANG Ping, CAI Shuihong, ZHAO Hongliang. Preparation and characterization of TOSPA complex[J]. CIESC Journal, 2010, 61(10): 2731-2737.
吴福忠, 龙中柱, 张平, 蔡水洪, 赵洪亮. TOSPA复合物的制备及其结构表征 [J]. 化工学报, 2010, 61(10): 2731-2737.
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