季铵化噻唑喹唑啉三碘化物的合成及其作为电位传感器活性物质的应用

D. Kut, Ye Mahada, M. Fershal, M. Kut
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引用次数: 0

摘要

首次合成、分离和鉴定了角三碘化物--1,2,4,5-四氢-4-乙基-1-(碘甲基)-1-甲基-5-氧代噻唑并[3,2-a]喹唑啉-10-鎓。元素分析证实了三碘化物的形成,含有融合噻唑啉环信号的核磁共振光谱也证实了其结构。环化过程通过信号倍率从单倍(硫醚)到双倍(噻唑)的变化以及甲基的光谱从 1.83 ppm 转移到 2.15 ppm 的较弱场得到了证实。找到了合成噻唑喹唑啉鎓三碘化物的最佳反应条件,即在氯仿中加入双过量碘,在室温下反应 24 小时,产率为 84%。传感器显示出 75 mV/pC 的超纳氏反应,I3- 的检测限为 5 10-6 mol/L,使用寿命超过 4 个月。该传感器对阴离子有选择性,对分子碘和碘化物有一定的敏感性。该传感器被用作指示电极,使用 KI3 溶液直接电位滴定颜色强烈的果汁和维生素制剂中的抗坏血酸。添加-发现法和高效液相色谱分析证实了其准确性。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
SYNTHESIS OF QUATERNIZED THIAZOLOQUINAZOLINIUM TRIIODIDE AND ITS APPLICATION AS AN ACTIVE SUBSTANCE FOR POTENTIOMETRIC SENSOR
For the first time, the synthesis, isolation, and identification of angular triiodide, 1,2,4,5-tetrahydro-4-ethyl-1-(iodomethyl)-1-methyl-5-oxothiazolo[3,2-a]quinazolin-10-ium, have been achieved. The formation of the triiodide was confirmed by elemental analysis, and its structure was approved by NMR spectra containing signals from the fused thiazolonine ring. The cyclization process was confirmed by the change in signal multiplicity from singlets (thioether) to doublets (thiazole) and a shift to a weaker field in the spectrum of the methyl group from 1.83 ppm to 2.15 ppm. Optimal reaction conditions for the synthesis of thiazolochinazolinium triiodide were found using a double excess of iodine in chloroform at room temperature for 24 hours, yielding 84%. The obtained thiazolochinazolinium triiodide product was utilized as an active substance for a PVC plasticized triiodide selective potentiometric sensor. The sensor exhibited a super-Nernstian response of 75 mV/pC with a detection limit of 5 10-6 mol/L I3- and a lifetime exceeding 4 months. The pH working range of the sensor was found to be within pH 2-10, with a response time of 15-30 s. The sensor is selective to anions and exhibits some sensitivity to molecular iodine and iodide. The sensor was used as an indicator electrode for the direct potentiometric titration of ascorbic acid using a solution of KI3 in intensely colored fruit juices and vitamin preparations. The accuracy was confirmed by the added-found  method and HPLC analysis.
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