Ti 2PbC was synthesized for the first time by pressureless reaction synthesis using Ti/Pb/TiC as starting materials at a heating rate of 2 ℃/min and holding at 1370 ℃ for 2 h in a tube furnace protected by Ar atmosphere. The effects of starting powders, heating rates, and holding temperatures on the formation of Ti 2PbC were investigated. It was found that elementary mixture of Ti/Pb/C or higher heating rates fail to form Ti 2PbC. The decreased lattice parameters in the synthesized Ti 2PbC indicated the existence of Pb vacancies in the compound. A reaction mechanism was proposed to explain the formation of Ti 2PbC.