The findings of this thesis are presented in four sections. First, diazotization and diazo coupling reactions of para-diazonium benzene sulfonyl azide with aromatic phenols over eco-friendly clay catalysts are described. These catalysts are inexpensive, noncorrosive and reusable. Also they have not considerable decreases in the efficiency after four cycles of operation. The new method totally avoids the use of acids, alkalies and toxic solvents in diazotization and diazo coupling reactions. After that the synthesis of a new diazo reactive dye containing 4-sulfonyl azide benzenediazonium salt with a variety of coupling components has been done. The coupling component used in this reaction are salicylic acid, methyl salicylate, ethyl salicylate, butyl salicylate, methyl 2,4-dihydroxy banzoate, ethyl 2,4-dihydroxy banzoateate, salicylamide, 2,4-dihydroxy bnanzamide, salicylaldhyde, salicylaldoxime, 2-hydroxyacetophenone respectively. The Structures of all of the compounds were confirmed by FT-IR, UV, 1 H NMR, 13 C NMR, mass spectroscopy and elemental analyses. Their solvatechromic properties in different solvents were also studied. Second, the thermal reaction of sulfonyl azide dye with cyclohexane, benzene, anisole, p -xylene, dihydropyran and pyridine was studied. Third, diazotization and diazocoupling reaction of para- amino benzene sulfonyl azide and para -amino benzene sulfonyl amide with cyclic amines with various ring sizes has been done. The cyclic amines used in these reactions are pyrrolidine, piperidine, 4-methylpiperidine, N-methylpiperazine, morpholine and hexamethyleneimine over eco-friendly clay catalysts. Finally, The structure and electronic properties of synthesized compounds in previous sections have been investigated theoretically at the level of AM1, PM3, and HF, DFT using the standard 6-31 G * basis set. The optimized structure, electronic properties, vibrational frequencies and relative energies of the molecules were obtained. Observed frequencies obtained from the IR spectrum of each compound have been compared with those calculated from theoretical results. The observed spectra were found to be in good agreement with the calculations. The effect resonance, conformation and ring size of cyclic amine on the ?-conjugation of triazenes were investigated.