四川农业大学学报 ›› 2016, Vol. 34 ›› Issue (01): 110-114,120.doi: 10.16036/j.issn.1000-2650.2016.01.020

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4-二甲氨基吡啶催化合成贝诺酯

李霞辉, 张伟, 龚永平, 赵谨, 夏寒玉, 王志刚, 李川川, 舒刚   

  1. 四川农业大学动物医学院, 四川 温江 611130
  • 收稿日期:2015-12-29 发布日期:2016-02-29
  • 通讯作者: 舒刚,硕士生导师,主要从事中药药理与药剂研究工作,E-mail:dyysg2005@sicau.edu.cn。 E-mail:dyysg2005@sicau.edu.cn
  • 作者简介:李霞辉,在读硕士研究生
  • 基金资助:
    四川省科技厅项目苗子工程(035Z1143)

4-Dimethylaminopyridine-catalyzed Synthesis of Benorilate

LI Xia-hui, ZHANG Wei, GONG Yong-ping, ZHAO Jin, XIA Han-yu, WANG Zhi-gang, LI Chuan-chuan, SHU Gang   

  1. College of Veterinary Medicine, Sichuan Agricultural University, Wenjiang 611130, Sichuan, China
  • Received:2015-12-29 Published:2016-02-29

摘要: [目的] 探索4-二甲氨基吡啶(DMAP)催化合成贝诺酯的方法。[方法] 利用DMAP与二环己基碳二亚胺(DCC)合成酯类化合物的优点,产物通过高效液相色谱法(HPLC)和红外光谱检测(IR)鉴定。[结果] 通过单因素试验探讨了反应温度,反应时间,原料比例,脱水剂用量和催化剂用量对目标物产率的影响,并通过正交试验设计法,优化工艺条件。所得最佳工艺条件为:DMAP:阿司匹林=5:100(%),DCC:阿司匹林=0.8:1.1(摩尔比),反应温度为40℃,反应时间为5h,根据正交试验结果对所得最佳条件进行3次平行试验,平行试验的平均产率为51%。[结论] 本试验结果表明,筛选的最终方法与我国通用生产方法相比,操作过程简单,反应温度无论是实验还是生产中都容易满足,整个反应过程安全易控,本方法是一种新的工艺路线,能够为生产提供理论依据。

关键词: 贝诺酯, 4-二甲氨基吡啶(DMAP), 二环己基碳二亚胺(DCC), 正交优化

Abstract: [Objective] In order to explore the method of 4 dimethylaminopyridine(DMAP) catalytic synthesis for benorilate. [Method] Used the advantagesof DMAP and N, N'-dicyclohexylcarbodiimide(DCC) synthesis esters, and identified the products by the HPLC and IR. [Results] Used the single factor experiment to discuss the effects of reaction temperature, reaction time, raw material ratio, catalyst dosage and the amount of dehydrating agent for the impact on target yield. And optimize process conditions by orthogonal test. Optimal condition is DMAP:Aspirin=5:100(%), the mole ratio of DCC and Aspirinis 0.8:1.1, reaction temperature 40℃, reaction time 5h, according to the results of orthogonal test 3 parallel tests were conducted. The average yield of parallel test was 51%. [Conclusion] The experiment results show that the final screening method compared with the general method of production, has some advantages like simple operation process, reaction temperature are easily satisfied both in experiment and production, and the reaction process is safety and easy to control. This method is a new process, to provide a theoretical basis for the production.

Key words: Benorilate, 4-dimethylaminopyridine-catalyze(DMAP), Dicyclohexylcarbodiimide(DCC), orthogonal test

中图分类号: 

  • 0652.3