Lignin-derived　monomers　with　methoxy　substituents　are　abundantly　present　in　bioliquids　derived　from　lignocellulosic　biomass.　Examples　are　the　products　obtained　from　the　reductive　catalytic　fractionation　of　lignin　(RCF)　and　pyrolysis　of　lignocellulosic　biomass　and　hydrotreated　products　thereof.　An　attractive　valorization　step　for　these　liquids　involves　demethoxylation　to　obtain　alkylated　phenols　through　selective　catalytic　hydrodeoxygenation　(HDO).　Within　the　context　of　sustainable　chemistry,　there　is　a　strong　drive　to　use　cheap,　non-precious　metal　catalysts　for　this　purpose.　In　this　study,　the　HDO　of　guaiacol　(5　wt%　in　toluene)　was　investigated　in　a　continuous　fixed-bed　reactor　at　380　°C,　20　bar　over　supported　MoO3　catalysts.　MoO3　(5　%)　supported　on　TiO2　(P25)　was　shown　to　give　superior　performance　compared　with　MoO3　supported　on　anatase　TiO2,　Al2O3,　SiO2,　Nb2O5,　CeO2,　and　ZrO2.　Additional　studies　involving　variation　of　the　Mo　loading　and　process　conditions　were　performed,　and　the　highest　selectivity　to　demethoxylated　phenolics　like　phenol　and　methylated　phenols　was　82　%　at　97　%　conversion　of　guaiacol.　Both　4-n-propylguaiacol　and　a　realistic　guaiacols-rich　feed　isolated　from　a　representative　pyrolysis　oil　were　also　successfully　demethoxylated　with　the　5　%　MoO3/TiO2　catalyst.　©　2022　The　Authors.　ChemCatChem　published　by　Wiley-VCH　GmbH.