The reaction between arylsulfonyl chlorides and hydrazine has been studied, and it has been found that in the presence of excess hydrazine, the bis-derivatives are produced in small amounts along with monoarylsulfonyl hydrazides. It has been revealed that the reaction of monosulfonyl hydrazides with alkyl bromides in the presence of a base results only in N-alkylation of the sulfamide nitrogen, although the reaction in the presence of HCl proceeds at the amine group with the formation of quaternary ammonium salts. A method for the preparation of sulfonyl hydrazides by oxidation of N-alkyl sulfamides in the presence of iodine has been developed. Some arylsulfonyl hydrazide derivatives have been examined as antioxidant, antirust, and antiwear additives. These sulfonyl hydrazides also exhibit a high bactericidal and fungicidal activity.