摘要
3-羟基-4-甲氧基苯丙烯醛,是合成新型高倍甜味剂爱德万甜(Advantame)的关键中间体。本文以强碱催化,使3-羟基-4-甲氧基苯甲醛和乙醛发生羟醛缩合反应,利用响应面法建立中间体得率与乙醛滴加时间、反应温度和NaOH浓度之间的数学模型,通过此模型确定中间体的最佳合成工艺参数,并采用紫外、红外、质谱和X射线衍射法(XRD)对中间体进行结构表征。结果表明:最佳工艺参数为乙醛滴加时间2 h、反应温度-5℃,NaOH浓度12%,在此条件下,中间体得率达61.28%±1.37%,与回归模型预测值64.75%基本相符。经紫外、红外、质谱和XRD光谱分析证实,合成产物即为甜味剂Advantame中间体3-羟基-4-甲氧基苯丙烯醛。
Advantame was a novel sweetener,3-hydroxy-4-methoxy benzal acrolein was a key intermediate to synthesize the sweetener.In this paper,3-hydroxy-4-methoxy benzal acrolein was synthesized via the reaction of 3-hydroxy-4-methoxy benzaldehyde and acetaldehyde under strong alkaline condition. The mathematical model of the yield of intermediate with reaction temperature, aldehyde dropwise time and alkali concentration was established by response surface methodology.Through this model, optimum synthetic process parameters were determined. Compositions of the products were characterized by UV, F＇FIR, MS and XRD.Resuhs showed that the optimized reaction conditions were 2 h,-5 ℃ and 12% for reaction temperature, aldehyde dropwise time and alkali concentration.Under these conditions, the intermediate productivity could reach 61.28% ± 1.37% ,which was accordance with the predicted data （64.75%）.The synthetic product was the intermediate of advantame through the analysis of UV, FFIR, MS and XRD.
作者
陈博儒
陈良
朱思明
CHEN Bo-ru;CHEN Liang;ZHU Si-ming(School of Food Science ＆ Engineering,South China University of Technology,Guangzhou 510640,China;Shandong Ben Yue bio-technology Co.,Shandong 257000,China;School of Life and Geography,Kashi University,Xinjiang 834000,China)
出处
《食品工业科技》
CAS
CSCD
北大核心
2018年第22期144-149,共6页
Science and Technology of Food Industry
基金
国家自然科学基金(U1203183)
关键词
甜味剂中间体
3-羟基-4-甲氧基苯丙烯醛
合成
响应面法
结构表征
sweetener intermediate
3- hydroxy-4 - methoxy benzal acrolein
synthesis
response surface methodology
structuralcharacterization
