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Selective Synthesis of a Salt and a Cocrystal of the Ethionamide-Salicylic Acid System

机译：选择性合成盐和乙酰胺 - 水杨酸体系的盐酸盐

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摘要

Herein is presented a rare example of salt/cocrystal polymorphism involving the adduct between ethionamide (ETH) and salicylic acid (SAL). Both the salt and cocrystal forms have the same stoichiometry and composition and are both stable at room temperature. The synthetic procedure was successfully optimized in order to selectively obtain both polymorphs. The two adducts' structures were thoroughly investigated by means of singlecrystal X-ray diffraction, solid-state NMR spectroscopy, and density functional theory (DFT) calculations. From the solidstate NMR point of view, the combination of mono- and multinuclear experiments (H-1 MAS, C-13 and N-15 CPMAS, H-1-{N-14} D-HMQC, H-1-N-14 PM-S-RESPDOR) provided undoubted spectroscopic evidence about the different positions of the hydrogen atom along the main N center dot center dot center dot H center dot center dot center dot O interaction. In particular, the H-1-N-1(4) PM-S-RESPDOR allowed N-H distance measurements through the H-1 detected signal at a very high spinning speed (70 kHz), which remarkably agree with those derived by DFT optimized X-ray diffraction, even on a natural abundance real system. The thermodynamic relationship between the salt and the cocrystal was inquired from the experimental and computational points of view, enabling the characterization of the two polymorphs as enantiotropically related. The performances of the two forms in terms of dissolution rate are comparable to each other but significantly higher with respect to the pure ETH.
机译：本文介绍了含盐/共聚物多态性的罕见实施例，涉及乙醇（Eth）和水杨酸（SAL）之间的加合物。盐和聚碳酸盐形式具有相同的化学计量和组合物，并且在室温下稳定。成功优化了合成程序，以选择性地获得两种多晶型物。通过单次X射线衍射，固态NMR光谱和密度泛函（DFT）计算彻底研究了两种加合结构。从固体NMR的角度来看，单核和多核实验的组合（H-1MAS，C-13和N-15 CPAMS，H-1- {N-14} D-HMQC，H-1-N- 14 PM-S-RESPDOR）提供了毫无疑问的光谱证据，沿着主N中心点中心点中心点H中心点中心点中心点O相互作用提供了关于氢原子的不同位置的光谱证据。特别地，H-1-N-1（4）PM-S-RESPDOR通过H-1检测到的信号以非常高的纺丝速度（70kHz）允许NH距离测量，这与DFT优化的那些非常同意X射线衍射，即使在天然丰富的真实系统上。从实验和计算的观点中寻找盐和碳库之间的热力学关系，使得两种多晶型物表征在对抗性相关的情况下。在溶解速率方面，两种形式的性能彼此相当，但相对于纯Eth均显着更高。

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  • 来源
    《Crystal growth & design》 |2020年第2期|共10页
  • 作者

    Bernasconi Davide; Bordignon Simone; Rossi Federica; Priola Emanuele; Nervi Carlo; Gobetto Roberto; Voinovich Dario; Hasa Dritan; Nghia Tuan Duong; Nishiyama Yusuke; Chierotti Michele R.;

  • 作者单位

    Univ Torino Dept Chem Via Giuria 7 I-10125 Turin Italy;

    Univ Torino Dept Chem Via Giuria 7 I-10125 Turin Italy;

    Univ Torino Dept Chem Via Giuria 7 I-10125 Turin Italy;

    Univ Torino Dept Chem Via Giuria 7 I-10125 Turin Italy;

    Univ Torino Dept Chem Via Giuria 7 I-10125 Turin Italy;

    Univ Torino Dept Chem Via Giuria 7 I-10125 Turin Italy;

    Univ Trieste Dept Chem &

    Pharmaceut Sci Piazzale Europa 1 Via L Giorgieri 1 I-34127 Trieste Italy;

    Univ Trieste Dept Chem &

    Pharmaceut Sci Piazzale Europa 1 Via L Giorgieri 1 I-34127 Trieste Italy;

    RIKEN SPring 8 Ctr NMR Sci &

    Dev Div Yokohama Kanagawa 2300045 Japan;

    RIKEN SPring 8 Ctr NMR Sci &

    Dev Div Yokohama Kanagawa 2300045 Japan;

    Univ Torino Dept Chem Via Giuria 7 I-10125 Turin Italy;

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  • 中图分类 晶体学;
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