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SPE–TLC Profiling of Impurities in 1-(3,4-Methylenedioxyphenyl)-2-nitropropene, an Intermediate in 3,4-Methylenedioxy- methamphetamine (MDMA) Synthesis

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Abstract

Impurity profiling of 1–(3,4-methylenedioxyphenyl)-2-nitropropene, an intermediate in the synthesis of 3,4-methylenedioxymethamphetamine (MDMA), has been studied by SPE combined with TLC. Extraction of impurities was performed on C18 columns. TLC separation was performed on 0.2 mm silica gel 60 plates, with fluorescent indicator F254, in a horizontal developing chamber. To improve the quality of the profile (increase the TLC sensitivity) SPE extracts were concentrated by evaporation in a stream of nitrogen. The usefulness of methanol, ethanol, ethyl acetate, chloroform, acetonitrile, and their mixtures as mobile phases was tested by use of Gibbs’s triangle. Spots of the separated impurities were observed under UV light (λexc=254 and 366 nm). The proposed characteristics of profile quality (optimization criteria) are based on matrix presentation of the TLC pattern. They take into account, simultaneously, the number of spots revealed, differences between RF values, and the intensity of fluorescence.

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Acknowledgments.

This study was partly supported by grant OT 00C 01024 from the Committee for Scientific Research, Poland.

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Authors and Affiliations

  1. Department of Analytical Chemistry, Faculty of Chemistry, Jagiellonian University, Ingardena 3, 30-060, Cracow, Poland

    J. Kochana & A. Parczewski

  2. Department of Organic Chemistry, Faculty of Chemistry, Jagiellonian University, Ingardena 3, 30-060, Cracow, Poland

    J. Wilamowski

  3. Institute of Forensic Research, Westerplatte 9, 31-033, Cracow, Poland

    A. Parczewski

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  1. J. Kochana
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  2. J. Wilamowski
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  3. A. Parczewski
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Correspondence to J. Kochana.

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Kochana, J., Wilamowski, J. & Parczewski, A. SPE–TLC Profiling of Impurities in 1-(3,4-Methylenedioxyphenyl)-2-nitropropene, an Intermediate in 3,4-Methylenedioxy- methamphetamine (MDMA) Synthesis. Chromatographia 60, 481–484 (2004). https://doi.org/10.1365/s10337-004-0385-7

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  • DOI: https://doi.org/10.1365/s10337-004-0385-7

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