1Introduction Sulfonyl hydrazide and sulfonyl semicarbazide derivatives exhibit variety of bactriostatic activity and also are important compounds as blowing agents in cellular rubber and plastics[1]. Different methods for the preparation of these compounds are reported for example, sulfonyl semicarbazides are prepared by reaction of a sulfonyl hydrazides with urea or cyanic acid[2], reaction of sulfinic acid salt with azodicarbonamide in water[3],and reaction of sulfonyl chloride and semicarbazide[4]. In lots of these methods the yields are not high, the solvents are toxic (pyridine)[5] and also the starting materials are not commericaly available[6]. We now report a modified and convenient procedure for the preparation of these compounds under solvent-free condition.