摘要
研究了盐酸戊乙奎醚工艺杂质的合成工艺,以便对盐酸戊乙奎醚的质量进行控制。以α-环戊基扁桃酸甲酯为起始原料,经还原、磺酰化、缩合、成盐等反应制备了工艺杂质3-[2-环戊基-2-苯基-2-(2-环戊基-2-羟基-2-苯基-乙氧基)乙氧基]奎宁环烷盐酸盐。目标产物的化学结构经质谱和氢谱确证,产品纯度为99.9%,总收率为16.7%(以α-环戊基扁桃酸乙酯计)。该工艺反应条件温和、操作简便,为盐酸戊乙奎醚的工艺杂质合成提供了一种新选择。
The synthetic process of impurities in penehyclidine hydrochloride was studied in order to control the quality of penehycli- dine hydrochloride. 3-[2-cyclopentyl-2-phenyl-2-（2-hydroxyl-2-cyclopentyl-2-phenylethoxy） ethoxy] quinuclidine hydrochloride was synthesized from methyl a-cyclopentyl-a-hydroxybenzeneacetate （2） as raw matercial via the reduction, sulfonylation, condensation and salification,etc. The chemical structure of the target product was confirmed by MS and 1H-NMR. The results showed that the to-tal purity was 99. 9% ,and the total yield was 16. 7%. The reaction condition was mild and the operation was simple,which provided a new choice for the synthesis of the impurity of penehyclidine hydrochloride.
出处
《化学研究与应用》
CSCD
北大核心
2017年第7期1079-1082,共4页
Chemical Research and Application
基金
海南省自然科学基金项目(814287)资助
国家级大学生创新实验项目(201511810003)资助
海南医学院大学生创新实验项目(HYCX2014007)资助
关键词
盐酸戊乙奎醚
抗胆碱药
工艺杂质
penehyclidine hydrochloride
anticholine drug
process impurity
