泊沙康唑主环的单晶制备及其结构表征

目的制备泊沙康唑主环的单晶,并对其进行结构表征和稳定性研究。方法通过溶剂挥法及气相扩散法制备出泊沙康唑主环的单晶,采用差示扫描量热仪(DSC)、粉末X射线衍射仪(PXRD)和单晶X射线衍射仪(SXRD)对其结晶形态进行表征。结果上述方法均可制备泊沙康唑主环单晶,其DSC和PXRD图谱一致,即晶型一致。SXRD结果表明泊沙康唑主环不对称单位化学计量式为C_(21)H_(21)F_2N_3O_4S,相对分子质量为449.47,晶体密度为1.408 g/cm~3,该晶胞属于单斜晶系,空间群为P2_1。均浆稳定性实验结果表明,不同极性溶剂中得到的晶体PXRD图谱未发生变化。结论实验确证了泊沙康唑主环的立体构型,且稳定性良好。

Single crystal preparation and structure confirmation of posaconazole main ring

Objective To prepare single crystals of posaconazole main ring, and to investigate the corresponding structure and thermodynamic stability. Methods Evaporation and vapor diffusion methods were used to grow single crystals of posaconazole main ring, which were then characterized by differential scanning calorimetry (DSC), powder X-ray diffraction (PXRD), and single X-ray diffraction (SXRD). Results Single crystals of pasaconazole main ring could be grown by the two methods, and the DSC curves and PXRD spectra of each sample were all consistent. SXRD results showed that the asymmetric unit stoichiometric of pasaconazole main ring was C₂₁H₂₁F₂N₃O₄S, relative molecular mass were 449.47, and crystal density were 1.408 g/cm³. The unit cell belonged to the monoclinic system, and the space group was P2₁. The slurry experiment results showed that PXRD spectra of posaconazole main ring suspended in different polar solvents were consistent. Conclusion Crystal structure of posaconazole main ring is characterized, and posaconazole main ring has good corresponding thermodynamic stability.