吡啶类离子液体催化乙酸冰片酯合成的工艺研究  

Study on the Synthetic Process of Bornyl Acetate Catalyzed by Pyridine Type Ionic Liquid

作　　者：刘永谦[1] 谢梓杰 钟洋均 刘付伟清 王涛[2] LIU Yongqian;XIE Zijie;ZHONG Yangjun;LIUFU Weiqing;WANG Tao(Department of Pharmacy,Guangdong Women and Children Hospital,Guangzhou 511442 Guangdong,China;School of Pharmaceutical Sciences,Guangzhou University of Chinese Medicine,Guangzhou 510006 Guangdong,China;Department of Gynecology,Guangdong Women and Children Hospital,Guangzhou 511442 Guangdong,China)

机构地区：[1]广东省妇幼保健院药学部,广东广州511442 [2]广州中医药大学中药学院,广东广州510006 [3]广东省妇幼保健院妇科,广东广州511442

出　　处：《中药新药与临床药理》2023年第7期970-975,共6页Traditional Chinese Drug Research and Clinical Pharmacology

基　　金：国家自然科学基金资助项目(30701100);广州中医药大学“双一流”与高水平大学学科协同创新团队项目(2021xk87)。

摘　　要：目的优化乙酸冰片酯的合成工艺,探索离子液体在酯化反应中的应用,为发展乙酸冰片酯的绿色合成工业提供参考。方法基于文献分析,设计、合成了吡啶类离子液体,并探讨其应用于酯化反应的可能性。采用响应面法的Box-Behnken试验设计,通过数学模型优化合成工艺。试验以乙酸冰片酯的收率为指标,进行单因素试验,考察不同反应物投料比、反应时间、催化剂用量的影响;在此基础上,利用响应面法进行多因素试验,建立数学模型进行寻优计算,得到各因素的最佳组合;最后进行验证试验。结果合成乙酸冰片酯的最佳条件为:冰片和乙酸酐质量比为1∶3,反应时间为11 h,催化剂用量为冰片质量的10%。验证试验所得实际收率为85.10%,与预测值接近。结论吡啶类离子液体作为催化剂,催化活性高、易分离、对环境友好,本合成工艺具有操作简单、原料易得、产品收率高、反应条件温和的特点,具有重要的应用价值。Objective To optimize the synthetic process of bornyl acetate and to explore the application of pyridine type ionic liquid in esterification.The study provides a reference for the development of green synthetic industry of bornyl acetate.Methods Based on the analysis of literature,pyridine type ionic liquid was designed and synthesized,and the possibility of its application in esterification was discussed.Then the Box-Behnken experimental design of the response surface method was used.The synthetic process was optimized by the statistical and mathematical model.Taking the yield of bornyl acetate as the index,we carried out the single factor test and investigated the effects of different reactant ratio,reaction time,and catalyst dosage.The comprehensive follow-up multi-factor test was carried out by using the response surface method,the mathematical model was established for optimization calculation,and the best combination of various factors was obtained.Finally,the verification test was conducted.Results The optimum conditions for the synthesis of bornyl acetate were as follows:the molar ratio of borneol to acetic anhydride was 1∶3,the reaction time was 11 hours,the amount of catalyst was 10% of the mass of borneol.The actual yield of the verification test was 85.10%,which was close to the predicted value.Conclusion It had been found that ionic liquid as a catalyst was applied in synthesis,which has high catalytic activity,easy separation,and environmental friendliness.The synthetic process has the characteristics of simple operation,easily available materials,high product yield,and mild reaction conditions.It has important application value.

关 键 词：乙酸冰片酯 离子液体 催化剂 响应面法 合成工艺 

分 类 号：R283.6[医药卫生—中药学]