文献类型：期刊文献

中文题名：异海松酸甲酯的合成与结构表征

英文题名：Synthesis and Structural Characterization of Methyl Isopimarate

作者：王迷霞[1] 徐士超[1,2] 卢言菊[1,2] 袁晓敏[1] 陈玉湘[1,2] 赵振东[1,2]

第一作者：王迷霞

通信作者：Zhao, Zhen-Dong

机构：[1]中国林业科学研究院林产化学工业研究所生物质化学利用国家工程实验室国家林业局林产化学工程重点开放性实验室江苏省生物质能源与材料重点实验室;[2]中国林业科学研究院林业新技术研究所

年份：2015

卷号：35

期号：6

起止页码：15-20

中文期刊名：林产化学与工业

外文期刊名：Chemistry and Industry of Forest Products

收录：CSTPCD;;EI(收录号：20161202132612);Scopus(收录号：2-s2.0-84960961119);北大核心:【北大核心2014】；CSCD:【CSCD2015_2016】；

基金：国家自然科学基金资助项目(31370575);中国林科院林业新技术所基本科研业务费专项基金(CAFINT2013C01)

语种：中文

中文关键词：异海松酸;异海松酸甲酯;合成;表征

外文关键词：isopimaric ; methyl isopimarate ; synthesis ; characterization

分类号：TQ35

摘要：以异海松酸为原料,草酰氯为酰氯化试剂,合成异海松酸酰氯活性中间体,在三乙胺作用下进行甲酯化反应制备异海松酸甲酯,并通过FT-IR、GC-MS、1H NMR和13C NMR等手段对产物进行了表征。用单因素试验法分别对异海松酸酰氯和异海松酸甲酯合成工艺进行优化,研究结果表明,当酰氯化反应中异海松酸与草酰氯物质的量比为1∶1,反应时间为3 h,甲酯化反应中异海松酸酰氯与三乙胺物质的量比为1∶0.24,反应时间为80 min时,目标产物的酰基转化率为99.43%,产物为白色晶体,总产率86.3%。
With isopimaric acid as initiating material, oxalyl chloride as the acyl chlorination reagent, isopimaric chloride active intermediate was synthesized. Then under the action of triethylamine, isopimaric chloride was reacted with methanol to obtain methyl isopimarate,and the title compound was characterized by FT-IR, GC/MS, IH NMR and 13C NMR spectroscopy. By single fraction tests ,the influences of reaction time, material ratio, and dosage of triethylamine on these two reactions were explored. The results showed that the optimal synthetic conditions of the reaction were the molar ratio of isopimaric acid and oxalyl chloride 1 ： 1, reaction time 3h in acyl chlorination reactoin, and the molar ratio of triethylamine and isopimaric chloride 1 ： 0.24, reaction time 80min in esterification reaction. Under these conditions, the acyl conversion rate was 99.43 %, the target product was white crystal and the total yield was 86.3 %.