The direct introduction of an amino acid into an isothiocyanate intermediate in an organic solvent is challenging, even at elevated temperatures, because of the low solubility of amino acids. However, when the amino acid and isothiocyanate intermediate are sonicated together for one hour, the amino acid dissolves, enabling the preparation of acylthioureas. Two acylthiourea compounds (1, 2) containing amino acid moiety have been prepared from the conventional preparation method incorporated with the ultrasonication process. The ultrasound has been utilized to dissolve the amino acid in the reaction mixture in anhydrous acetone solvent and to initiate the formation of amino acid incorporated acylthiourea derivative. The synthesis was carried out between benzoyl chloride, potassium thiocyanate and an amino acid (serine or proline) in anhydrous acetone solvent. The acylthioureas were obtained in good yields and isolated in high purity. The elemental analysis, UV–vis, FT–IR and 1H & 13C–NMR spectroscopic methods have been used to characterize the prepared acylthiourea derivatives. The molecular structure of the synthesized compounds 1 and 2 was analyzed by SCXRD (single-crystal X-ray diffraction) method. Extensive computational analyses, including DFT calculations, Hirshfeld surface analysis, and energy framework analysis, were performed to understand the electronic properties and solid-state supramolecular features.
Titanocene (III) chloride mediated deiodination reaction of benzyl iodide has been reported. The reaction proceeds through the formation of benzyl radical. The benzyl radical reacts with another benzyl radical to afford a bibenzyl product. Also, the radical can be trapped using one electron deficient double bond. Titanocene(III) chloride has been generated by reduction of titanocene dichloride using activated zinc dust in deoxygenated THF under argon condition. As Ti(III) is a single electron donor, it can readily reduce the active iodo compound to form the corresponding carbon radical, which further reacts with appropriate functionality to obtain the desired product.
In this study, a potentiometric sensor based on a glyphosate–tetraphenylborate (GP–TPB) ion pair was developed for the selective detection of glyphosate. The GP–TPB material structure was investigated using FTIR analysis. The analytical performance of the sensor was systematically evaluated with respect to potentiometric response, detection limit, repeatability, pH dependence, and selectivity. The developed sensor exhibited a wide linear working range from 5.90 × 10-3 to 5.90 × 10-7 M, with a low detection limit of 9.37 × 10-9 M. The sensor demonstrated good stability and reproducibility at glyphosate concentrations of 5.90 × 10-4, 5.90 × 10-5, and 5.90 × 10-6 M, and maintained stable potentiometric performance over a broad pH range of 5–11. Selectivity studies confirmed a preferential response toward glyphosate in the presence of common interfering species. The applicability and accuracy of the proposed sensor were validated through comparative LC–MS/MS analyses. The results indicate that the GP–TPB-based potentiometric sensor provides a simple, rapid, and sensitive approach for glyphosate determination, with potential applicability in environmental and food sample analysis.
