Coupling In Situ Time-Resolved FTIR and Microwave Irradiation: Application to the Monitoring of Quinoxaline Derivatives Synthesis

The dataset supports a study focused on the development and optimisation of a green synthetic methodology for quinoxaline derivatives using microwave-assisted synthesis combined with in situ FTIR spectroscopy for real-time reaction monitoring. The investigated model reaction is the microwave-assisted condensation of benzil with 1,2-phenylenediamine leading to 2,3-diphenylquinoxaline.The dataset contains time-resolved in situ FTIR spectroscopic data and derived kinetic profiles collected under varied experimental conditions, including different catalytic systems (hydrochloric acid and molecular iodine) and solvents. These data enable comparative evaluation of reaction kinetics, catalyst efficiency, and solvent effects.Additionally, the dataset includes structural characterisation data of the final product, comprising NMR, MS, and IR spectra of 2,3-diphenylquinoxaline. The dataset is intended to support reproducibility, quantitative kinetic analysis, and further methodological development in microwave-assisted green synthesis.The ATR-FTIR Nicolet iS50 Tri-Detector Gold Flex Spectrometer (Thermo Scientific, Waltham, MA, USA) was employed to monitor the reaction’s course and analyse the obtained products. This spectrometer features a wave number range of 9600–20 cm−1 with an interferometer speed of 65 scans/s and separability of 16 cm−1. Additionally, the spectrometer is equipped with a fibre optic probe. The spectral results were obtained and processed via Omnic software (Series 9.12.928). The wavenumber area 1900–600 cm−1 was used for analysis in all experiments.