A series of low-loaded metallic-activated carbon catalysts were evaluated during the selective hydrogenation of a medium-chain alkyne under mild conditions. e catalysts and support were characterized by ICP, hydrogen chemisorption, Raman spectroscopy, temperature-programmed desorption (TPD), temperature-programmed reduction (TPR), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR micro-ATR), transmission electronic microscopy (TEM), and X-ray photoelectronic spectroscopy (XPS). When studying the effect of the metallic phase, the catalysts were active and selective to the alkene synthesis. NiCl/C was the most active and selective catalytic system. Besides, when the precursor salt was evaluated, PdN/C was more active and selective than PdCl/C. Meanwhile, alkyne is present in the reaction media, and geometrical and electronic effects favor alkene desorption and so avoid their overhydrogenation to the alkane. Under mild conditions, nickel catalysts are considerably more active and selective than the Lindlar catalyst.