This study reports a viable method for the synthesis of Ti2SC phase using iron disulfide or iron sulfide as sulfur source and a post-treatment with acid. The reaction routes to Ti2SC phases starting from two different chemical compositions of 2Ti-FeS2-2TiC and Ti-FeS-TiC were in detail explored and compared through the analysis of X-ray diffraction, thermogravimetry/differential scanning calorimetry, and scanning electron microscopy results. Unlike the Ti-FeS-TiC composition, the reaction route from 2Ti-FeS2-2TiC composition contained an extra decomposition step in which FeS2 transformed to activated FeS and released molecular state sulfur at temperature around 500 degrees C. The latter at this temperature could successfully trigger the reaction of Ti-S-TiC to form Ti2SC phase, which was an analogous self-propagating high-temperature synthesis with a high transient temperature. On the contrary, only trace of Ti2SC phase could be obtained at temperature as high as 1200 degrees C from the Ti-FeS-TiC composition. The main impurity phases from these iron disulfide reactant systems were Fe and FeS, and they could be easily purified by dissolution in H2SO4 solution, which resulted in Ti2SC phase with a minor TiC phase in the final product.