三氯蔗糖-6-乙酸酯的合成及其工艺优化  

Synthesis and Process Optimization of Sucralose-6-acetate

作　　者：冷一欣[1] 刘晓成[1] 苏继光[1] 张云[1] 武玉真[1] 黄成龙[1] 万屹东 

机构地区：[1]常州大学石油化工学院,江苏省绿色催化材料与技术重点实验室,江苏常州213164 [2]常茂生物化学工程股份有限公司,江苏常州213034

出　　处：《食品科学》2013年第22期106-110,共5页Food Science

摘　　要：用SOCl2和N,N-二甲基甲酰胺(DMF)合成Vilsmeier试剂,氯化蔗糖-6-乙酸酯制得三氯蔗糖-6-乙酸酯,并经IR、1H NMR确认其结构。考察投料物质的量比、向反应体系中所添加甲苯的比例、还原反应过程中pH值及氯代温度。结果表明:在80℃条件下最适宜制备Vilsmeier试剂;n(Vilsmeier试剂):n(蔗糖-6-乙酸酯)=11:1,m(甲苯):m(DMF)=1:10,还原反应中pH7.5;反应分3个阶段,一氯代在70℃、二氯代在90℃、三氯代在110℃最适宜进行氯代反应;合成三氯蔗糖-6-乙酸酯收率达到55.7%。Sucrose-6-acetate was chlorinated in the presence of Vilsmeier reagent, which was synthesized with SOC12 and DMF. The structure of the sucralose-6-acetate obtained was confirmed by IR and IH NMR. Chlorination temperature, the molar ratio of reaction substrates, the amount of toluene added and pH in the reduction reaction were optimized. The most suitable temperature to prepare the Vilsmeier reagent was 80 ℃. The molar ratio of Vilsmeier reagent to sucrose-6-acetate was 1l：1 and mass ratio of toluene to N,N-dimethylformamide was 1：10. The optimized pH was 7.5 in the reduction reaction. This chlorination reaction was divided into three steps with three chlorination temperatures of 70, 90 ℃ and 110 ℃, respectively. The yield of sucralose-6-acetate under the optimized reaction conditions was 55.7%.

关 键 词：蔗糖-6-乙酸酯 三氯蔗糖-6-乙酸酯 Vilsmeier试剂 氯代 

分 类 号：TS202.3[轻工技术与工程—食品科学]