3-氨基-1-金刚烷醇合成工艺的优化  

Optimization of the preparation process of 3-amino-1-adamantane alcohol

作　　者：张豪 张明[1] 李毓飞 纪雯鹏 李儒清 王天宝 胡湘南[1] ZHANG Hao;ZHANG Ming;LI Yufei;JI Wenpeng;LI Ruqing;WANG Tianbao;HU Xiangnan(Department of Pharmacy, Chongqing Medical University, Chongqing,400016, P. R. China)

机构地区：[1]重庆医科大学药学院

出　　处：《华西药学杂志》2018年第3期227-230,共4页West China Journal of Pharmaceutical Sciences

基　　金：重庆市科委资助项目(cstc2015zdcy-ztzx120003);重庆医科大学大学生科学研究与创新实验项目(201616)

摘　　要：目的制备维格列汀重要中间体3-氨基-1-金刚烷醇,并优化其制备工艺。方法以盐酸金刚烷胺为原料,用混酸反应、碱解的方法制得3-氨基1-金刚烷醇粗品,后处理过程中首次采用乙醇进行提取,并应用星点设计-效应面法优化该工艺参数。结果所制备化合物的结构经IR、1HNMR、13CNMR、MS确证;收率可达95%,纯度97.66%。结论优化后的工艺稳定、可行,具备一定实际应用价值,适合工业化生产。OBJECTIVE To prepare the key intermediate of Vildagliptin：3 - amino - 1 adamantane alcohol and to optimize the preraration process. METHOD The crude product of 3 - amino - 1 - adamantanol was prepared by the reaction of acid and alkaline solution based on amantadine hydrochloride. The extraction process was carried out for the first time in the post - treatment process, in which the process parameters were optimized by Central composite design - response surface methodology. RESULTS The structure of the synthesized componds was confirmed by IR,1HNMR,13CNMR and MS. The yield was 95% and the purity was 97.66%. CONCLUSION The optimized process is stable and feasible, and has certain practical application value, which is suitable for indus- trial production.

关 键 词：维格列汀 3-氨基-1-金刚烷醇 合成 中间体 星点设计-效应面法 工艺优化 

分 类 号：R914[医药卫生—药物化学]