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Liquid Crystals and their Application
Russian Journal Zhidkie kristally i ikh prakticheskoe ispol'zovanie Жидкие кристаллы и их практическое использование |
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Zhidk. krist. ikh prakt. ispol'z. = Liq. Cryst. and their Appl., 2015, 15 (1), 28—33. |
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Use of Gas-Liquid Chromatography for Separation of Alkylation Products of 3,5-Diamino-1,2,4-Triazoles – Precursors of Macroheterocyclic Compounds
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T. E. Dubrovina, T. V. Kudayarova, E. A. Danilova
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Author affiliations
Research Institute of Macroheterocycles,
Ivanovo State University of Chemistry and Technology,
7 Sheremetevsky Ave., Ivanovo, 153000, Russia
E-mail: danilova@isuct.ru
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Abstract
1N-Alkyl-3,5-diamino-1,2,4-triazoles possess mesomorphic properties. We developed a new purification method for alkyl-3,5-diamino-1,2,4-triazoles, consisting in the extraction of the free base of alkylguazole by chloroform, further recrystallization of the final product from toluene, scrubbing of the impurities on the filter with hexane, repeated recrystallization from toluene and final column chromatography (silica gel, hexane/ethyl acetate = 1:3). The developed method of purification allows to separate 1N-alkyl-3,5-diamino-1,2,4-triazole from a mixture of other products of alkylation effectively. The compounds were characterized by mass-spectrometry, IR- and NMR- spectroscopy and elemental analysis.
Keywords: synthesis, 1-alkyl-3,5-diamino-1,2,4-triazole, macroheterocyclic compounds, mesomorphic properties
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