Methodology is reported for the synthesis of a six-membered heterocyclic ring involving cyclocondensation reaction through sulfur-sulfur bond formation. This method of synthesis allows for developing a new class of dithiadiazines. A series of bis-[6-tetra-O-acetyl-β-D-glucopyranosylimino-1,2,4-triazolo[3,4-b]-1,2,4,5-dithiadiazin-4-yl] alkanes have been synthesized by using a reagent, tetra-O-acetyl-β-D-glucopyranosylimino chloromethane sulfenyl chloride and bis-(4-amino-5-mercapto-1,2,4-triazol-3-yl) alkanes. These newly formulated N-glycosylated molecules could serve as a potential biological entity.