In the present study, the synthesis of titanium nitride (TiN) by carbothermal reduction nitridation (CRN) reaction using nanocomposites made of mesoporous TiO2/acrylonitrile with different content of inorganic phase were explored. The choice of hybrid nanocomposite as precursor for the synthesis of TiN was made due to the possibility of having an intimate interface between the organic and inorganic phases in the mixture that can favours CRN reaction. Subsequently, the hybrid composites have been subjected to four-step thermal treatments at 290 °C, 550 °C, 1000 °C and 1400 °C under nitrogen atmosphere. The XRD results after thermal treatment at 1000 °C under nitrogen flow show the coexistence of two crystalline phases of TiO2, i.e. anatase and rutile, as well as TiN phase, together with the detection of amorphous carbon that proved the initiation of CRN reaction. Furthermore, the observations based on XRD patterns of samples thermally treated at 1400 °C in nitrogen atmosphere were in agreement with SEM analysis, that shows the formation of TiN by CRN reaction via hybrid nanocomposites mesoporous TiO2/acrylonitrile.