盐酸普拉克索B晶型的制备和表征

    Preparation and Characterization of Form B of Pramipexole Dihydrochloride

    • 摘要: 目的 制备盐酸普拉克索的B晶型并优化制备工艺,同时进行结构表征和稳定性研究。方法 制备盐酸普拉克索的B晶型,采用热重法(TGA)、差示扫描量热法(DSC)、X射线粉末衍射(PXRD)、X射线单晶衍射(SXRD)等分析手段,对盐酸普拉克索B晶型进行表征研究。结果 制备得到了盐酸普拉克索B晶型,其晶型属正交晶系,空间群P212121,结构中不含溶剂(包括水)。盐酸普拉克索B晶型热处理后晶型不发生转变。结论 盐酸普拉克索B晶型为无水晶型,热稳定性优于一水合物晶型,具有高温稳定性。

       

      Abstract: OBJECTIVE To obtain the new preparation method of polymorphic form B of pramipexole dihydrochloride and discuss it’s thermodynamics stability and crystal structure. METHODS Polymorphic form B of pramipexole dihydrochloride was characterized by thermal gravimetric analysis(TGA), differential scanning calorimetry(DSC), powder X-ray diffraction(PXRD) and single crystal X-ray diffraction(SXRD). RESULTS Preparation method, crystal structure and polymorphic stability of polymorphic form B of pramipexole dihydrochloride was obtained. The results showed that form B was in the orthorhombic space group P212121 with formula C10H19Cl2N3S as the anhydrous form. pramipexole dihydrochloride form B was more stable than pramipexole dihydrochloride monohydrate form in high temperature condition. CONCLUSION Form B of pramipexole dihydrochloride is anhydrous which is more stable at high temperature. Form B has good stability at high temperature.

       

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