Mo–Si–Al–C-based multiphase compounds and their composites reinforced by micro-SiC and TiC particulates were manufactured by means of reactive hot-pressed sintering method. Their microstructure and room temperature mechanical properties were studied. The results showed that Al addition and the ratio of Si/Al exerted a remarkable effect on the reaction products in the Mo–Si–Al–C systems. For the stoichiometric Mo 5(Si,Al) 3C mixed powders with a molar ratio of Mo:Si:Al:C as 5:1.5:1.5:1, the sintered body contained Mo 3Si, Mo 3Al 2C, and Mo 5Si 3C as the major reaction products whereas and the minor phases consisted of MoSi 2, Mo 2C, and Mo(Si,Al) 2 compounds. When the starting powder mixture was off-stoichiometric with a small amount of excess Si, only Mo 2C accounted for the minor product. Moreover, the relative contents of the former three major phases were affected by the changed Si/Al ratio, where the amounts of Mo 3Al 2C and Mo 5Si 3C compounds decreased and increased, respectively with increasing Si/Al ratio. The two multiphase alloys showed poor mechanical properties, due to the existence of residual porosity. In contrast, the composites exhibited superiority in both flexural strength and fracture toughness at room temperature to the Mo–Si–Al–C-based multiphase compounds. MSAC1/20 wt.%SiC and MSAC1/20 wt.%TiC composites had a respective flexural strength and fracture toughness of 454 and 438 MPa, 4.93 and 4.85 MPa m .