[关键词]
[摘要]
目的 寻找一条合成目标化合物4-(6-脱氧-β-D-吡喃葡萄糖基)-1-甲氧基-2-[(反式-4-正丙基环己基)甲基]苯的简易路线,并研究其晶型。方法 利用苯基溴化物片段和6-脱氧葡萄糖酸内酯片段作为起始原料合成目标化合物;采用有机混合溶剂和含水混合溶剂结晶的方式制备目标化合物的晶型,采用粉末X射线衍射分析和热重–差热分析技术对其进行表征,并对其进行了初步稳定性研究。结果 目标化合物的总收率为74%,通过上述制备方法获得了同一种晶型,该晶型对光、热和湿均是稳定的。结论 设计了一条合成目标化合物的简易路线,该路线操作简便、路线短、收率高,并制备了一种具有良好稳定性的目标化合物的晶型。
[Key word]
[Abstract]
Objective To search for a facile synthetic route for synthesis of target compound 4-(6-deoxy-β-D-glucopyranosyl)-1- methosyl-2-[(trans-4-n-propylcyclohexyl)methyl] benzene and to study its polymorphic characteristics. Methods A phenyl bromide fragment and 6-deoxygluconolactone fragment were used as starting materials to synthesize the target compound. Polymorph of target compound was prepared from organic mixed solvents and aqueous mixed solvents. and was characterized by powder X ray diffraction (PXRD), and thermogravimetric analysis coupled with differential thermal analysis (TG-DTA), and the preliminary stability properties of the polymorph was also studied. Results The total yield of target compound was 74%. The same polymorph of the target compound was obtained by the above methods, and was stable to light, heat, and moisture. Conclusion A facile synthetic route for synthesis of target compound is developed, which has the advantages of simple operating procedure, easy post-processing and high yield, and a stable polymorph of target compound is obtained.
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[基金项目]
国家自然科学基金资助项目(21302141);天津市科技计划项目(10ZCKFSH01300)