基于连续流微通道反应器合成盐酸金刚烷胺工艺研究  

Research on Synthesis of Amantadine Hydrochloride Based on Continuous Flow Microchannel Reactor

作　　者：杜芳琼 王渊 吴秋莹 徐丽萍[1,2] Du Fangqiong;Wang Yuan;Wu Qiuying;Xu Liping(Sichuan Vocational College of Chemical Industry,Luzhou 646300;The Key Laboratory of Fine Chemical Application Technology of Luzhou,Luzhou 646300,China)

机构地区：[1]四川化工职业技术学院,四川泸州646000 [2]精细化工应用技术泸州市重点实验室,四川泸州646000

出　　处：《广东化工》2023年第9期7-9,26,共4页Guangdong Chemical Industry

摘　　要：为解决传统釜式反应在盐酸金刚烷胺制备过程中存在的反应时间长、返混大等问题,通过连续流微通道反应器,以1-溴代金刚烷、尿素、盐酸等为原料对盐酸金刚烷胺进行了制备,其结构通过高分辨质谱(HRMS)和核磁氢谱(1H NMR)得到了证明。进而对其制备条件进行了考察,重点考察了反应物料摩尔比、停留时间、反应温度、反应压力等影响因素对产物产率的影响。实验结果表明,实验条件下,当物料摩尔比为1∶4、反应温度为100℃、反应停留时间为15 min,产物产率可高达90%,为最佳工艺条件。该工艺极大地提高了此反应合成盐酸金刚烷胺的工艺转化率,为其工业化应用提供了技术指导。In order to solve the problems of long reaction time and large backmixing in traditional kettle reaction in the preparation of amantadine hydrochloride,amantadine hydrochloride was prepared by using 1-bromoadamantadine,urea,hydrochloric acid,etc.as raw materials through a continuous flow microchannel reactor,and its structure was proved by high resolution mass spectrometry(HRMS)and nuclear magnetic resonance(1H NMR).Then the preparation conditions were investigated,focusing on the effects of the molar ratio of reactants,residence time,reaction temperature,reaction pressure and other factors on the product yield.The experimental results showed that under the experimental conditions,when the molar ratio of materials was 1∶4,the reaction temperature was 100℃,and the reaction residence time was 15 min,the product yield could reach 90%,which was the optimal process condition.This process greatly improves the conversion rate of the reaction to synthesize amantadine hydrochloride,and provides technical guidance for its industrial application.

关 键 词：连续流 微通道 盐酸金刚烷胺 工艺 

分 类 号：TQ460.6[化学工程—制药化工]