Background/Objectives: Reference materials are essential for ensuring the accuracy and traceability of measurements in the quality control of medicinal products. This study explores new principles for the preparation of impure materials of active pharmaceutical substances, focusing on 1-(3-benzoylphenyl)ethanone ketoprofen impurity A (European Pharmacopoeia) as the reference material. Methods: The reference material was synthesised from commercially available acetanilide and benzoyl chloride. The obtained product was purified using preparative chromatography and characterised by infrared spectroscopy (IR), 1H and 13C nuclear magnetic resonance (NMR), and mass spectrometry. The structure was verified using primary research methods to confirm its identity as the target product. Results: The characterisation confirmed the structure and purity of 1-(3-benzoylphenyl)ethanone, achieving a purity of 99.86%, meeting regulatory documentation requirements. The synthesised product was demonstrated to be identical to the target compound and suitable for use as a reference material. Conclusions: The developed method provides a robust approach for the preparation and characterisation of 1-(3-benzoylphenyl)ethanone, enabling its use as a certified reference material in the quality control of medicinal products. This approach ensures compliance with regulatory standards and enhances the reliability of pharmaceutical quality assurance practices.

A two-stage synthesis of the novel compound 1-(1-methyl-5-thiocyanato-1H-pyrrol-2-yl)-3-nitro-1H-1,2,4-triazole utilizing electrochemistry as an environmentally benign tool is reported. The structure of the target molecule was confirmed by ¹H and ¹³C NMR spectroscopy and HRMS. The compound exhibits antibacterial and antifungal activity comparable to chloramphenicol, ciprofloxacin, and fluconazole.

In this work, we carried out a double C–H thiocyanation of 7-methoxy-1H-indole to afford the novel 7-methoxy-3,4-dithiocyanato-1H-indole in good yield. The structure of the target product was confirmed by ¹H and ¹³C NMR spectroscopy, FT-IR spectroscopy, and HRMS.