目的 培養(yǎng)(S)-2-(Boc-氨基)-3-[(S)-2-氧代-3-吡咯烷基]丙酸甲酯單晶，并進(jìn)行晶型表征和立體結(jié)構(gòu)確證。方法 用醋酸乙酯-甲基叔丁基醚（1∶1）體系培養(yǎng)單晶，并采用熱重法、差示掃描量熱法、粉末X射線衍射和單晶X射線衍射分析。結(jié)果 制備得到無(wú)色塊狀晶體；樣品熔點(diǎn)約為114 ℃；該晶胞屬于正交晶系，空間群為P2₁2₁2₁，分子式為C₁₃H₂₂N₂O₅，相對(duì)分子質(zhì)量為286.33，晶體密度為1.152 mg/mm³，絕對(duì)構(gòu)型為S,S構(gòu)型。結(jié)論 確定了(S)-2-(Boc-氨基)-3-[(S)-2-氧代-3-吡咯烷基]丙酸甲酯的立體構(gòu)型，培養(yǎng)的晶體為非水合物和溶劑化物。

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.

R914