The carbonylation at the benzyl C-Hal bonds (Hal = F, Cl) of a number of polyfluorinated alkylbenzenes and benzocycloalkenes using carbon monoxide in the presence of SbF₅ is described. The reaction provided the corresponding α-arylcarboxylic acids or their methyl esters following aqueous or methanol treatment. The products of double carbonylation were obtained from bis(chloromethyl)tetrafluorobenzenes and benzal fluorides. For benzal chloride derivatives, the possibility of selective mono- or dicarbonylation was shown to depend on the amount of antimony pentafluoride. In the case of polyfluorinated secondary benzyl halides with a hydrogen atom at the α-carbon atom and vicinal fluorine atoms, the addition of CO was found to be accompanied by the elimination of HF, resulting in α,β-unsaturated α-arylcarboxylic acids. The double elimination of HF during the carbonylation of 1,4-dichloro-2,2,3,3,5,6,7,8-octafluorotetralin yielded dimethyl perfluoronaphthalene-1,4-dicarboxylate.

The hydrogenation of the biomass platform compound, ethyl levulinate, for the synthesis of γ-valerolactone represents a highly promising pathway for biomass valorization. Transition metal phosphates are extensively utilized in biomass hydrogenation reactions due to their Brønsted and Lewis acid sites. In this study, we synthesized a series of transition metal (Ni, Co, and NiCo) phosphide catalysts using the liquid phase method. We investigated the effects of metal species and initial Co/Ni molar ratios on catalytic activity in hydrogenation of ethyl levulinate and optimized the reaction conditions. The NiCoP-1.00 sample, prepared with a Co/Ni molar ratio of 1, demonstrated high efficacy in the hydrogenation of ethyl levulinate to γ-valerolactone, achieving excellent selectivity (97.9%) under optimized conditions. Experimental findings indicate that the synergistic interaction between Ni and Co facilitates the hydrogenation of the intermediate ethyl 4-hydroxypentanoate to γ-valerolactone while inhibiting excessive hydrogenation. The catalytic performance of the NiCoP-1.00 catalyst remained stable over five recycling runs.