Abstract: By previously reported modified Masai-Rausch method for synthesizing titano-Cycles, followed by add hydrolysis, trisubstituted alkenes were synthesized, yields obtained were higher than that reported in literature.Starting from unsymmetrical alkyne substrates, twelve different types of substituted alkenes were synthesized, among which only two were found of single component, others were of isomer mixtures.Besides conventional analytical methods, NMRspectral analysis of titanocycle intermedlates and the products was used to identify the isomeric structures as well as their relative contents.