Dyes are organic compounds which gives colour to a substrate. Azo dyes are the largest group of colorants used in industry. Due to their ability to absorb visible light & ease of synthesis dyes have wider industrial application and use such as textiles, fiber, leather, print and painting, also in agriculture, cosmetics & in laboratories. In this research eight azo compounds are prepared by diazo coupling. The diazotizonium salt is formed when NaNO 2 & concentrated HCl is treated with substituted aromatic amines viz. Aniline, Anthranilic acid, α-Naphathalamine, Benzidene, o-Nitroaniline, p-nitroaniline, sulphanilic acid and ptoulidine. The formation of novel dye took place with a sufficient yield with subsequent coupling of 2,4-dimethylphenol. The structures of prepared dyes are confirmed by Fourier transform Infrared & proton nuclear magnetic resonance spectroscopy. Perkin Elmer spectrum used for IR spectra & Bruker Avance 400MHz NMR spectrometer for NMR spectra. The IR spectra showed 3000-3500cm-1 streching for hydroxyl group & 1405-1550cm-1 streching for-N=Nbond and mass of azo compound found to be m/z 304(M+).