[关键词]
[摘要]
目的 培养(S)-2-(Boc-氨基)-3-[(S)-2-氧代-3-吡咯烷基]丙酸甲酯单晶,并进行晶型表征和立体结构确证。方法 用醋酸乙酯-甲基叔丁基醚(1∶1)体系培养单晶,并采用热重法、差示扫描量热法、粉末X射线衍射和单晶X射线衍射分析。结果 制备得到无色块状晶体;样品熔点约为114 ℃;该晶胞属于正交晶系,空间群为P212121,分子式为C13H22N2O5,相对分子质量为286.33,晶体密度为1.152 mg/mm3,绝对构型为S,S构型。结论 确定了(S)-2-(Boc-氨基)-3-[(S)-2-氧代-3-吡咯烷基]丙酸甲酯的立体构型,培养的晶体为非水合物和溶剂化物。
[Key word]
[Abstract]
Objective To cultivate the single crystal and perform crystal morphology characterization and stereo-structural confirmation of methyl (S)-2-(tert-butoxycarbonyl) amino-3-[(S)-2-oxopyrrolidin-3-yl] propanoate. Methods The single crystals were cultivated with of ethyl acetate-methyl tert-butyl ether (1:1) solvent system, and TGA, DSC, XRPD, and SXRD were used to analyze. Results Nice colorless bulk crystals were obtained with approximately 114℃ of melting point. The crystal cell belongs to an orthogonal crystal system, with a spatial group of P212121. Molecular formula was C13H22N2O5, molecular weight was 286.33, crystal density was 1.152 mg/mm3, and an absolute configuration was S,S style. Conclusion The stereo-configuration of methyl (S)-2-(tert-butoxycarbonyl) amino-3-[(S)-2-oxopyrrolidin-3-yl] propanoate has been confirmed, and the cultured crystals are non-hydrated and solvated.
[中图分类号]
R914
[基金项目]