(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
Single crystal culture and its structure characterization of methyl(S)-2-(tert-butoxycarbonyl)amino-3-[(S)-2-oxopyrrolidin-3-yl]propanoate
许常旭 1杨海刚 1莫小鹏 1胡勇 1钱圣典 1邵建平 1王未 1张俊 1张强 1毛龙2
作者信息
- 1. 杭州艾森医药研究有限公司,浙江 杭州 310030
- 2. 艾森医药股份有限公司,美国 圣地亚哥 CA92121
- 折叠
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.
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.
关键词
(S)-2-(Boc-氨基)-3-[(S)-2-氧代-3-吡咯烷基]丙酸甲酯/单晶/热重法/差示扫描量热法/粉末X射线衍射/单晶X射线衍射/构型Key words
methyl(S)-2-(tert-butoxycarbonyl)amino-3-[(S)-2-oxopyrrolidin-3-yl]propanoate/single crystal/TGA/DSC/PXRD/SXRD/configuration引用本文复制引用
出版年
2024
NETL
NSTL
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