Identification and Physicochemical Characteristics of Temozolomide Process-Related Impurities

Molecules

Marta ᐚszcz¹  Marek Kubiszewski¹  Łukasz Jedynak¹  Monika Kaczmarska¹  Łukasz Kaczmarek¹  Wojciech Łuniewski¹  Krzysztof Gabarski¹  Anna Witkowska¹  Krzysztof Kuziak¹ 

[1] Pharmaceutical Research Institute (PRI), Warszawa 01-793, Poland; E-Mails:

关键词: temozolomide intermediate;    X-ray crystallography;    nuclear magnetic resonance;    high-performance liquid chromatography;   

DOI  :  10.3390/molecules181215344

来源: mdpi

【 摘 要 】

In this article the crystal structures of the starting material TZ-5 and the key intermediate TZ-6 of temozolomide (TZ-7), an anticancer therapeutic agent, are presented, together with their spectroscopic and thermal characteristics. Both compounds crystallize in the triclinic P-1 space group. X-ray crystallography studies proved that the compound TZ-6 exists as a monohydrate. A complete structural assignment was obtained for the signals in the ¹H-, ¹³C- and ¹⁵N-nuclear magnetic resonance spectra and the structures were confirmed by Fourier-Transform infrared and Raman spectroscopy. The article describes the importance of the high purity of TZ-6 during the small-scale plant production of TZ-7 in a desired polymorphic form III with the purity higher than 99.50%, according to an HPLC method.

【 授权许可】

CC BY   
© 2013 by the authors; licensee MDPI, Basel, Switzerland.