摘要
目的制备阿普斯特E晶型的单晶,并对其进行结构表征和稳定性研究。方法通过溶剂挥法制备出阿普斯特E晶型的单晶,采用差式扫描量热仪(DSC)、粉末X射线(PXRD)及单晶X射线仪(SXRD)对其进行表征,利用均浆实验对其晶型稳定性进行考察。结果乙腈溶剂挥发法可制备得到阿普斯特E晶型的单晶,其DSC和PXRD图谱与文献报道一致。SXRD结果表明阿普斯特E晶型的单位化学计量式为C_(22)H_(24)N_2O_7S,相对分子质量为460.49,晶体密度为1.262g/cm~3,该晶胞属于正方晶系,空间群为P4_12_12。均浆稳定性实验结果表明,不同极性溶剂中得到的晶体DSC图谱发生变化。结论实验确证了阿普斯特E晶型的立体构型,不同溶剂中晶型发生变化。
Objective To prepare single crystals of apremilast form E, and to investigate the corresponding structure and thermodynamic stability. Methods Evaporation method was used to grow single crystals of apremilast form E, which were then characterized using differential scanning calorimetry(DSC), powder X-ray diffraction(PXRD), and single X-ray diffraction(SXRD). Results Single crystals of apremilast form E could be obtained through acetonitrile evaporation. DSC graph and PXRD spectrum was in good agreement with data reported in literatures. SXRD results showed that the unit stoichiometric of apremilast form E was C_(22)H_(24)N_2O_7 S, and the relative molecular mass was 460.49, and crystal density was 1.262 g/cm~3. The unit cell belonged to a tetragonal system, and the space group was P4_12_12. The slurry experiment results showed that DSC graphs of apremilast samples suspended in different polar solvents were different. Conclusion Crystal structure of apremilast form E is characterized, and the crystallization changes in different solvents.
引文
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