This paper presents the study of a simple and fast method to prepare an activated hydrothermal carbon supported nickel electrocatalyst (Ni/aHC) for ethanol oxidation reaction (EOR) in alkaline medium. The cyclic voltammogram obtained for the Ni/aHC sample in a 1.0molL−1 NaOH solution shows an anodic and a cathodic peak. These redox couple reaction peaks can be related to the reversible formation of (NiO)OH. The catalytic activity of the Ni/aHC sample regarding the EOR is clearly evident from the cyclic voltammogram obtained in presence of ethanol, where a significant increase in the current density from 0.55V vs. Hg/HgO is observed. This potential value, related with the onset potential (Eonset) of the EOR, is very close to the corresponding (NiO)OH formation potential, confirming that this species is directly involved in the EOR on the Ni/aHC electrocatalyst. The in-situ Attenuated Total Reflectance FTIR (in-situ ATR-FTIRS) spectra of this sample show two intense peaks related with acetate ion formation. Based on the ATR-FTIRS and electrochemical analyses, and in the literature information, a reaction pathway of the EOR on Ni/aHC in alkaline medium is proposed.