The synthesis of some novel azo dye (II-VII) derivatives of substituted phenols have been carried out by reacting phenol, 2,6-dimethylphenol, 2-tert-butylphenol, 4-tert-butylphenol, 2-tert-butyl-4-methylphenol, and 2-tert-butyl-4-methoxyphenol with para-tert-butylaniline as a coupling component. The characterisation of these compounds has been described by IR, UV- VIS, H-1-NMR spectroscopic techniques, thin-layer chromatography, and elemental analysis.