文献类型：期刊文献

中文题名：草酸二龙脑酯的合成及其表征

英文题名：Synthesis and Characterization of Dibornyl Oxalate

作者：张平辉[1,2,3,4] 赵振东[1,2,3,4,5] 徐士超[1,2,3,4] 毕良武[1,2,3,4,5] 卢言菊[1,2,3,4,5] 李冬梅[1,2,3,4,5] 王迷霞[1,2,3,4] 袁晓敏[1,2,3,4]

第一作者：张平辉

机构：[1]中国林业科学研究院林产化学工业研究所;[2]生物质化学利用国家工程实验室;[3]国家林业局林产化学工程重点开放性实验室;[4]江苏省生物质能源与材料重点实验室;[5]中国林业科学研究院林业新技术研究所

年份：2014

卷号：31

期号：11

起止页码：1402-1405

中文期刊名：精细化工

外文期刊名：Fine Chemicals

收录：CSTPCD;;Scopus;北大核心:【北大核心2011】；CSCD:【CSCD2013_2014】；

语种：中文

中文关键词：龙脑;草酸二龙脑酯;表征;精细化工中间体

外文关键词：borneol ; dibornyl oxalate ; characterization ; fine chemical intermediates

分类号：TQ351.4

摘要：在偏钛酸或者硼酐催化作用下,龙脑和草酸发生酯化反应生成草酸二龙脑酯,探讨了催化剂类型及用量、原料配比、反应温度以及反应时间对酯化反应的影响。结果表明,在50.0 g正己烷溶剂中,m(龙脑)∶m(草酸)∶m(催化剂)=5.0∶12.0∶3.0,于55℃下反应96 h,龙脑的转化率及草酸二龙脑酯的选择性分别为95.8%和99.4%。通过HRMS、IR、1HNMR、13CNMR等对草酸二龙脑酯进行了鉴定与表征。
Dibornyl oxalate was synthesized from esterification reaction between borneol and oxalic acid catalyzed by metatitanic acid or boron anhydrous. The effect of reaction conditions such as selectivity and dosage of catalyst, material ratio, reaction temperature and reaction time on the conversion of borneol and product selectivity of dibornyl oxalate were explored. The results showed that the optimal synthetic conditions of this reaction were： mass ratio of borneol with anhydrous oxalic acid and catalyst 5.0∶12.0∶3.0, reaction temperature 55℃ and reaction time 96 h. Under the reaction conditions, the conversion rate of borneol and the selectivity of dibornyl oxalate were 95.8% and 99.4%, respectively. The structure of dibornyl oxalate was identified and characterized by HRMS, IR, 1H NMR and 13C NMR.