摘要
通过比较不同的反应路线,确定了以1,3-二甲基金刚烷为原料,经溴代、乙酰氨基化、水解反应最后经酸化得到盐酸美金刚胺。改进并优化了合成路线,溴代反应确定为在回流条件下反应12h,n(1,3-二甲基金刚烷)∶n(溴素)=1∶1.5;水解反应条件是以n(乙二醇)∶n(水)=10∶1为溶剂,150℃下反应12h,n(1-乙酰氨基-3,5-二甲基金刚烷)∶n(氢氧化钠)=1∶5,反应总收率达81.5%。产品用IR、ESI、1HNMR、13CNMR确证了产品的结构。
Comparing to different reaction methods, the method starting from 1,3-dimethyladamantane was certified with the memantine hydrochloride synthesized by bromination ,acetimidolation, hydrolysis and acidation.Bromination was run under reflux for 12h, molar ratio of 1,3-dimethyladamantane to bromine was l：l.5;hydrolysis was carried out with molar ratio of glycol to water 10：1 as solvent at 150℃ for 12h, molar ratio of 1-acetimdolyl-3,5-dimethyladmantane to sodium hydroxide was 1：5. The overall yield reached 81.5%.Structures of the product were characterized by IR,ESI,^1HNMR and ^13CNMR.
基金
山东省青年科学家基金
No.2005BS04009
关键词
盐酸美金刚胺
溴代
水解
优化
memantine hydrochloride
bromination
hydrolysis
optimization
