Ti2SC has been synthesized using Ti/TiS2/2TiC as initial materials. Combining X-ray diffaraction analysis with thermodynamic calculations, a reaction path is proposed for the intermediate phase TiS and Ti2SC formation. TiS was more possible to be obtained from TiS2 and Ti rather than the decomposition of TiS2. TiC was the main impurity phase in Ti2SC and was difficult to eliminate. The high pressure technology using can help improve the purity of the sample. Scanning electron microscopy (SEM) shows the typically layer structure of the material. Thermogravimetry (TG) and differential scanning calorimetry (DSC) are also to be used to investigate the reaction mechanism，indicating that it would be useful for the formation of more purity sample by adjusting the content of TiS2.