摘要
目的制备(S)-N-环氧丙基邻苯二甲酰亚胺的单晶,并对其进行结构表征和均浆稳定性研究。方法通过溶剂挥发法和气相扩散法制备(S)-N-环氧丙基邻苯二甲酰亚胺晶型。利用差示扫描量热仪(DSC)、热重分析仪(TGA),红外光谱仪(IR),粉末X射线衍射仪(PXRD)和单晶X射线衍射仪(SXRD)分别对制备得到的晶体样品进行表征。结果制备得到的(S)-N-环氧丙基邻苯二甲酰亚胺晶体样品,其DSC、TGA、IR和PXRD图谱均一致,即晶型一致;DSC结合TGA分析结果显示,(S)-N-环氧丙基邻苯二甲酰亚胺熔点为100.56℃,分解温度为128.2℃。单晶X射线衍射结果表明该晶胞属于单斜晶系,P2_1空间群,结构偏离因子R=0.04,分子式为C_(11)H_9NO_3,相对分子质量为203.19,立体构型与预测构型一致。均浆稳定性实验结果表明,不同极性溶剂中得到的晶体粉末X射线未发生变化,即晶型稳定性良好。结论实验确证了(S)-N-环氧丙基邻苯二甲酰亚胺的立体结构,且晶型稳定性良好。
Objective To grow crystals of（S）-N-glycidyl phthalimide and investigate the corresponding structure and thermodynamic stability. Methods Evaporation and vapor diffusion methods were applied to grow crystals of（S）-N-glycidyl phthalimide. Different analysis methods including differential scanning calorimetry（DSC）, thermogravimetric analysis（TGA）, infrared spectrometry（IR）, powder X-ray diffraction（PXRD）, and single X-ray diffraction（SXRD） were used to characterize the corresponding crystal structure. Results The DSC curves, TGA curves, IR spectra, and PXRD spectra of samples grown by the above methods were all consistent. Referring to the DSC and TGA results, the melting and decomposition temperatures were determined to be around 100.56 ℃ and 128.2 ℃, respectively. SXRD confirms the monoclinic lattice with space group P2_1 in（S）-N-glycidyl phthalimide crystal with a refinement value（R） of 0.04. Moreover, the chemical formula and relative molecular mass were C_（11） H_9 NO_3 and 203.19, respectively. The measured crystal structure was in good agreement with the predicted one. Further, slurry experiments, which were performed in different polar solvents, confirmed the stability of the solid state of（S）-N-glycidyl phthalimide based on the PXRD determination. Conclusion Crystal structure of（S）-N-glycidyl phthalimide is characterized and the corresponding thermodynamic stability is investigated.
作者
施珍娟
刘扬
姚莉丽
张亮
张相洋
SHI Zhen-juan;LIU Yang;YAO Li-li;ZHANG Liang;ZHANG Xiang-yang(State Key Laboratory of Chemical Engineering,East China University of Science and Technology,Shanghai 200237,China;Hisun Co.,Ltd.,Taizhou 318000,China)
出处
《现代药物与临床》
CAS
2018年第7期1555-1560,共6页
Drugs & Clinic
基金
国家自然科学基金资助项目(21406071)
作者简介
施珍娟（1981-），女，浙江金华人，工程师，主要从事药物分析及药物晶型研究。E-mail：zjshi@hisunpharm．com;通信作者张相洋E-mail：zxydcom@ecust．edu．cn
