Vilsmeier试剂合成及其制备三氯蔗糖-6-乙酯的机理研究  

Study on Synthesis of Vilsmeier Reagent and the Mechanism of Preparation of Sucralose-6-ethyl ester

作　　者：童惠姗 TONG Huishan(Zhejiang Pharmaceutical University,Ningbo,Zhejiang 315100,China)

机构地区：[1]浙江药科职业大学,浙江宁波315100

出　　处：《浙江化工》2025年第4期15-20,共6页Zhejiang Chemical Industry

摘　　要：三氯蔗糖-6-乙酯是新型甜味剂三氯蔗糖的重要中间体,以氯化亚砜(SOCl_(2))与N,N-二甲基甲酰胺(DMF)为原料合成Vilsmeier试剂,Vilsmeier试剂氯化蔗糖-6-乙酯得到三氯蔗糖-6-乙酯。考察了SOCl_(2)与DMF的质量比、温度、搅拌速度和含水量等因素对Vilsmeier试剂合成的影响,探讨Vilsmeier试剂制备三氯蔗糖-6-乙酯的反应机理。结果表明:SOCl_(2)与DMF的质量比为1:2.5、温度为-2℃、搅拌速度在120~150 r/min之间合成的Vilsmeier试剂氯化效果最佳;反应体系中含水量超过1.0 wt%时合成的Vilsmeier试剂氯化效果较差。采用最优参数制备的Vilsmeier试剂氯化蔗糖-6-乙酯得到的三氯蔗糖-6-乙酯总收率达到47.8%。Sucralose-6-ethyl ester is an important intermediate of the new sweetener sucralose.Vilsmeier reagent is synthesized from sulfoxide chloride(SOCl_(2))and N,N-dimethylformamide(DMF).Sucrose 6-ethyl ester is chlorinated by Vilsmeier reagent to obtain sucralose-6-ethyl ester.In this paper,the effects of mass ratio of SOCl_(2) to DMF,temperature,stirring speed,and water content on the synthesis of Vilsmeier reagent were investigated,and the reaction mechanism of Vilsmeier reagent to sucralose-6-ethyl ester was discussed.The results showed that the chlorination effect of Vilsmeier reagent was the best when the mass ratio of SOCl_(2) to DMF was 1:2.5,the temperature was -2℃,and the stirring speed was 120~150 r/min.When the water content in the reaction system exceeded 1.0 wt%,the synthesized Vilsmeier reagent had poor chlorination effect.The total yield of sucralose-6-ethyl ester synthesized by chlorination of Vilsmeier reagent prepared with optimal parameters reached 47.8%.

关 键 词：三氯蔗糖-6-乙酯 SOCl_(2) Vilsmeier试剂 温度 转速 含水量 

分 类 号：TS202.3[轻工技术与工程—食品科学]