微通道中3-氨基-1-金刚烷醇的连续流工艺  

Continuous Synthesis Process of 3-amino-1-adamantane Alcohol in Microreactor

作　　者：毛苏雅 MAO Su-ya(Huai'an High Tech Research Institute of Nanjing University,Jiangsu Huaian 223005,China)

机构地区：[1]南京大学淮安高新技术研究院,江苏淮安223005

出　　处：《广州化工》2023年第24期119-120,124,共3页GuangZhou Chemical Industry

摘　　要：3-氨基-1-金刚烷醇是糖尿病治疗药物维格列汀的关键起始物料。在微反应器中,由1-金刚烷胺先硝化再水解连续合成3-氨基-1-金刚烷醇。考察了1-金刚烷胺与硝酸的摩尔比、反应温度、反应时间等对原料转化率、选择性和杂质的影响,并优化了相关工艺参数。结果表明,反应温度60℃,硝酸/1-金刚烷胺摩尔比为2.27,硝酸/1-金刚烷胺质量比为0.76,反应时间2.1 min, 1-金刚烷胺单程转化率达98.4%,选择性92.5%。与传统间歇釜式反应工艺相比,微通道反应工艺提高了的收率和选择性,缩短了反应时间,减少了原料消耗,实现了连续化操作,提高了生产安全性。3-amino-1-adamantanol is a key starting material for the treatment of diabetes drug viggliptin.In a Microreactor,3-amino-1-adamantanol was synthesized by nitration and hydrolysis of 1-amantadine amine.The effects of molar ratio of 1-amantadine to nitric acid,reaction temperature and reaction time on the conversion,selectivity and impurities of raw materials were investigated,and the relevant process parameters were optimized.The results showed that the reaction temperature was 60℃,the molar ratio of nitric acid to amantadine was 2.27,the mass ratio of nitric acid to amantadine was 0.76,and the reaction time was 2.1 min.The one-way conversion rate of 1-amantadine was 98.4%,and the selectivity was 92.5%.Compared with the traditional batch reactor reaction process,the microchannel reaction process improved the yield and selectivity,shortened the reaction time,reduced the consumption of raw materials,realized the continuous operation,and improved the production safety.

关 键 词：微通道反应器 3-氨基-1-金刚烷醇 1-金刚烷胺 

分 类 号：O657.3[理学—分析化学]