【摘要】 目的:分离及合成盐酸氨溴索原料药中的杂质反式四氢喹唑啉环己醇盐酸盐(DHTQ)。方法:通过柱层析分离出盐酸氯溴索原料中的杂质DHTQ;以盐酸氨溴索为原料,经过甲醛水溶液环化一步合成DHTQ。结果:分离并首次合成了DHTQ,结构经核磁共振氢谱、碳谱、质谱、红外光谱和元素分析确证,为盐酸氨溴索的质量标准检查提供了对照品。结论:该合成方法简单方便,收率高。更多还原

【Abstract】 Objective:To synthesis and separate DHTQ（6,8-dibromo-3-（trans-4-hydroxy cyclo- hexyl）-1,2,3,4-tetrahydroquinazoline）,an impurity of ambroxol hydrochloride. Methods:DHTQ was separated as an impurity from the raw material ambroxol by a column chromatographic procedure.Starting from ambroxol hydrochloride,DHTQ was prepared via cyclization reaction with formaldehyde（37% a- queous solution）.Results:The structure of DHTQ was verified using ¹H-NMR,¹³C_NMR,MS,IR and elemental analysis.Conclusion:The improved synthetic route offered an easy way to produce the refer- ence sample DHTQ for the quality control of ambroxol.更多还原