(S)-2-(Boc-氨基)-3-[(S)-2-氧代-3-吡咯烷基]丙酸甲酯单晶制备及其结构表征

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。

Single crystal culture and its structure characterization of methyl (S)-2-(tert-butoxycarbonyl) amino-3-[(S)-2-oxopyrrolidin-3-yl] propanoate

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.