This　paper　deals　with　a　study　of　the　mechanism　of　hydrodeoxygenation　(HDO)　at　0.1　MPa　and　300-350　°C　of　2-methyltetrahydrofuran　(2-MTHF)　over　a　Ni2P/SiO2　catalyst.　The　study　was　conducted　using　in　situ　Fourier　transform　infrared　(FTIR)　spectroscopy　to　monitor　the　adsorbed　species　during　reaction　and　in　situ　X-ray　absorption　fine　structure　(XAFS)　to　probe　the　oxidation　state　of　the　Ni　component.　The　work　is　relevant　to　the　upgrading　of　bio-oil　derived　from　the　pyrolysis　of　biomass.　It　was　deduced　that　the　initial　interaction　of　the　2-MTHF　was　with　OH　groups　on　the　catalyst　surface,　followed　by　adsorption　on　Ni　sites.　Ring-opening　of　the　tetrahydrofuran　led　to　the　formation　of　the　main　products　of　the　reaction,　n-pentane　by　HDO　and　n-butane　+　CO　by　decarbonylation.　The　CO　band　appeared　with　a　slight　delay　in　the　FTIR　spectrum　because　the　reaction　to　form　n-pentane　was　favored　and　turned　over　about　four　times　before　one　n-butane　+　CO　was　formed.　Copyright　©　2018　American　Chemical　Society.