[關(guān)鍵詞]
[摘要]
目的 尋找一條合成目標化合物4-(6-脫氧-β-D-吡喃葡萄糖基)-1-甲氧基-2-[(反式-4-正丙基環(huán)己基)甲基]苯的簡易路線,并研究其晶型。方法 利用苯基溴化物片段和6-脫氧葡萄糖酸內(nèi)酯片段作為起始原料合成目標化合物;采用有機混合溶劑和含水混合溶劑結(jié)晶的方式制備目標化合物的晶型,采用粉末X射線衍射分析和熱重–差熱分析技術(shù)對其進行表征,并對其進行了初步穩(wěn)定性研究。結(jié)果 目標化合物的總收率為74%,通過上述制備方法獲得了同一種晶型,該晶型對光、熱和濕均是穩(wěn)定的。結(jié)論 設(shè)計了一條合成目標化合物的簡易路線,該路線操作簡便、路線短、收率高,并制備了一種具有良好穩(wěn)定性的目標化合物的晶型。
[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.
[中圖分類號]
[基金項目]
國家自然科學(xué)基金資助項目(21302141);天津市科技計劃項目(10ZCKFSH01300)