摘要
本文报道了应用相转移催化技术合成中间体邻乙氧基苯酚及产物乙基香兰素,考察了反应温度、时间、物料配比等因素对合成的影响,确立了优化条件。同时采用 UV,IR,~1HNMR 和 GC方法对产物进行表征。研究结果显示聚乙二醇相转移催化合成邻乙氧基苯酚,叔胺相转移催化合成乙基香兰素结果满意。邻乙氧基苯酚最高收率达74.5%,乙基香兰素最高收率达73.5%。另外,还对反常 Reimer-Tiemann 反应相转移催化合成乙基香兰素的机制进行了讨论。
In this paper,the systematic research of synthesizing intermediate o- ethoxyphenol and terminal product ethylvanillin by phase-transfer-catalysis technique has been reported.We have investigated the intersection effection of several interrelat- ed factors such as reaction temperature,reaction time and mixing ratio of reactants, found,out the regularity and obtained the optimal conditions.Results indicate that synthesizing o-ethoxyphenol by using PEG as phase-transfer-catalyst and synthesiz- ing ethylvanillin by tertiary amine are satisfactory.The yield of o-ethoxyphenol reach up to 74. 5% and ethylvanillin 73. 5%.In addition,we preliminarily explore the mechanism of abnormal Reimer-Tiemann reaction for synthesizing ethylvanillin by phase transfer catalysis.
出处
《合成化学》
CAS
CSCD
1993年第4期333-340,共8页
Chinese Journal of Synthetic Chemistry
关键词
乙基香兰素
相转移催化
食用香料
o-Ethoxyphenol
Ethylvanillin
Phase-transfer-catalysis
Sythesis
PEG
Tertiary amine
Reaction mechanism
Reimer-Tiemann reaction