At various temperatures, real time FTIR analysis was introduced to monitor the kinetics of the uncatalyzed Huisgen 1,3-dipolar azide-alkyne cycloaddition (AAC) without media, resulting in in situ robust polymeric networks crosslinked with triazoles at chain-ends. Second-order kinetic analysis was used to determine the rate constants for uncatalyzed AAC reaction. Electron-deficient alkynes carrying an a-carbonyl undergo a fast Huisgen reaction within a few hours without any catalysts, proportional to the temperature. Less electron-deficient alkynes led to the decrease of AAC reaction rate significantly, revealing that the AAC reaction rate depends on the molecular structure of alkynes center