摘要
三氯蔗糖是性能最为优良的高甜度甜味剂之一。蔗糖-6-乙酸酯的选择性氯化是合成三氯蔗糖的关键步骤。蔗糖酯化合成的蔗糖-6-乙酸酯,不经纯化,经适当处理直接进入氯化阶段,用氯化亚砜与DMF预先生成的Vilsmeier试剂对其进行氯化,该方法具有收率高、操作简便及后处理容易等特点。优化的工艺条件为反应温度115℃,SOCl2与蔗糖-6-乙酸酯的摩尔比10∶1,DMF(mL)与蔗糖-6-乙酸酯(g)之比12∶1及反应时间3h。对中间产物三氯蔗糖-6-乙酸酯,经熔点测定、IR及1H-NMR确认了结构。
Sucralose is a kind of high intensity sweetener with significant characteristics. Selecting chlorination of hydroxyl group in sucrose 6-acetate is a key in the process of making sucralose. Sucrose-6-acetate, prepared by using triethyl orthoacetate without crystallization, could be chlorinated by Vilsmeier reagent which was subjected thionyl chloride to DMF. This method had many advantages: high yield, easy operation and easy process. Optimum condition was: reaction temperature 115℃, the mole ratio of SOCl2 and sucrose 6- acetate 10:1, the ratio of DMF(mL) and sucrose 6-acetate(g)12:1, reaction time 3h. The structure of the last compound was confirmed by using melting point mensuration, IR and^1H-NMR.
出处
《食品科技》
CAS
北大核心
2007年第3期158-161,共4页
Food Science and Technology