Chemistry Department, Faculty of Science, Narain (P.G.) College, Shikohabad-205 135, Uttar Pradesh, India Manuscript received 15 May "2009, revised 26 August 2009, accepted 28 October 2009 An efficient and extremely fast procedure to synthesize novel biologically active substituted trlnuoro-2-azetldones heterocycles was discussed. Reaction of trifluoroacetic hydrazide 2 with hydrazine hydrate and then cyclization with tetramethoxy methane yields N-(3-(trifluoromethyl)-5-methozy-4H-1,2,4-triazol-4-yl)amine 3. Condensation of the N-(3· (trifluoromethyl)-5-methozy-4H-1,2,4-trlazol-4-yl)amine 3 with corresponding aldehydes yields Schiff base (4a-k). Reaction of Schiff base with chloroacetyl chloride yields the corresponding substituted 3-chloro-1-(3-(trifluoromethyl)-5-methoxy-4H-1,2,4-triazol-4-yl)-4-pbenylazetidin-2-one (5a-k).