期刊
SOLID STATE NUCLEAR MAGNETIC RESONANCE
卷 122, 期 -, 页码 -出版社
ACADEMIC PRESS INC ELSEVIER SCIENCE
DOI: 10.1016/j.ssnmr.2022.101820
关键词
API; Polymorphs; X-ray diffraction; MAS NMR; Dynamics; Quantum mechanics calculations; DFT-D; GIPAW
资金
- European Research Space (PL-GRID) [04.04.00-00-4374/17-01]
- European Union under the European Regional Development Fund [04.04.00-00-4374/17-01]
- Regional Operational Program of the Lodz Region [RPLD.01.01.00-10-0008/18]
This study investigated new salts of teriflunomide with inorganic counterions using techniques such as solid-state NMR spectroscopy, X-ray diffraction, and single crystal X-ray diffraction. The results showed a conformational change in the teriflunomide molecule in the crystalline salt structures, forming an intramolecular hydrogen bond.
New salts of teriflunomide TFM (drug approved for Multiple Sclerosis treatment) with inorganic counterions: lithium (TFM_Li), sodium (TFM_Na), potassium (TFM_K), rubidium (TFM_Rb), caesium (TFM_Cs) and ammonium (TFM_NH4) were prepared and investigated employing solid state NMR Spectroscopy, Powder X-ray Diffraction PXRD and Single Crystal X-ray Diffraction (SC XRD). Crystal and molecular structures of three salts: TFM_Na (CCDC: 2173257), TFM_Cs (CCDC: 2165288) and TFM_NH4 (CCDC: 2165281) were determined and deposited. Compared to the native TFM, for all crystalline salt structures, a conformational change of the teriflunomide molecule involving about 180-degree rotation of the end group, forming an intramolecular hydrogen bond N-H?O is observed. By applying a complementary multi-technique approach, employing 1D and 2D solid state MAS NMR techniques, single and powder X-ray diffraction measurements, as well as the DFT-based GIPAW calculations of NMR chemical shifts for TFM_Na and TFM_Cs allowed to propose structural features of TFM_Li for which it was not possible to obtain adequate material for single crystal X-Ray measurement.
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