Aims: To synthesis new compounds via condensation reactions between 2-methyl quinoxaline-1,4-dioxide derivatives 4,4'-biphenyl carboxaldehyde. Methodology: The Quinoxalines derivatives were prepared from 2-nitroaniline derivatives using the Beirut reaction, and the condensation reaction was carried out at room temperature in absolute methanol. Based on IR and NMR spectroscopic techniques, the structures of all products have been suggested. For their synthesis, suitable mechanisms have been suggested. Results: In this work, condensation reactions involving 2-methyl quinoxaline-1,4-dioxide derivatives and 4,4'-biphenyl carboxaldehyde were performed. Conclusion: The final compounds, we suppose, have considerable applications in fluorescent and chromophoric activities. In all known solvents, the products were just slightly soluble. Products have been subjected to sulfonation reactions, although with limited success.