一种盐酸萘甲唑啉工艺杂质的制备及表征  

Preparation and Characterization of an Process Impurity of Naphazoline Hydrochloride

作　　者：蔚建勇 石均平 魏海涛 朱正兵 王恒南 安运懿 陈颖江 Wei Jianyong;Shi Junping;Wei Haitao;Zhu Zhengbing;Wang Hengnan;An Yunyi;Chen Yingjiang(API Division,Shanxi,Xi'an Taikomed Pharmaceutical Technology Co.,Ltd.,Xi'an 710076,China;R&D Department,Hebei Wuluo Pharmaceutical Co.,Ltd.,Hengshui 053500,China)

机构地区：[1]西安泰科迈医药科技股份有限公司原料药事业部,陕西西安710076 [2]河北武罗药业有限公司研发部,河北衡水053500

出　　处：《山东化工》2024年第18期64-65,共2页Shandong Chemical Industry

摘　　要：目的:描述了盐酸萘甲唑啉原料药合成过程中产生的一个工艺杂质(API-ZE):N,N′-1,2-乙烷二烷基双(1-萘乙酰胺)的制备和精制。方法:目标杂质(API-ZE)是在高温条件下,以α-萘乙酸(2)和乙二胺(3)为起始原料,通过氨解反应得到。结果:目标杂质的结构经^(1)H NMR、^(13)C NMR和HR-MS谱进行了确证,纯度达到99%(HPLC)以上。结论:此工艺杂质的成功获得,使盐酸萘甲唑啉的杂质研究更加全面和深入,为其工艺放大和质量控制提供了保障。This paper described the synthesis and refine of a process impurities N,N'-1,2-ethanediylbis-(1-Naphthaleneacetamide)(API-ZE),produced during the synthesis process of naphazoline hydrochloride.The target impurity(API-ZE)was synthesized withα-naphthaleneacetic acid(2)and ethylenediamine(3)as starting materials under high-temperature aminolysis.The target impurities structure was confirmed by^(1)H NMR,^(13)C NMR,and HR-MS spectrum,and the purity is up to 99%(HPLC).The successful obtaining of the impurity makes the impurity study of naphthalazoline hydrochloride more comprehensive and in-depth,and provides a guarantee for its process amplification and quality control.

关 键 词：盐酸萘甲唑啉 工艺杂质 氨解反应 

分 类 号：TQ460.6[化学工程—制药化工]