Sulfonamide drugs are those that contain an SO2-NH2 moiety. The class includes several groups of drugs used in the treatment of bacterial infections, diabetes mellitus, edema, hypertension, and gout. In this study, spectrometric analysis to identify the structures of some new sulfonamide forms and preparation of compounds by chlorosulfonylation of the diazonium salt though Sandmeyer reaction. The reaction procedure was simple and yields of target products were good.