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In this book deals with fast and efficient synthesis of arylazoxy Sulfides from Tribenzene Sulphenamide derivatives. Using this methodology we have successfully synthesized 17 derivatives of aryl azoxy sulfides of benzodioxane and also we have demonstrated fast and high yielding method for the preparation of arylazoxy sulfides using aryl nitraso compounds and tribenzenesulphenamide derivatives. Moreover the dioxolane ring on nitraso compounds resembles the frame work belongs to Calvatic acid derivative. Hence our research work may useful in further development of arylazoxy sulfide related molecules and their biological activities.