The objectives fixed by world’s governments concerning energy transition have aroused interest on lignocellulosic biomass utilization for bioenergy and green chemistry applications. However, due to their resistant structure, deconstructive pretreatments are necessary to render possible biological conversions of these lignocellulosic residues. Microwave (MW) treatment has been reported as efficient in many biotechnology fields; biomass pretreatment for biorefinery purposes is another possible application. This work presents the effects of MW pretreatment on underexploited natural agri-food biomass of economic interest: wheat bran, miscanthus stalks and corn stalks. Various parameters were studied including solvent, power density, treatment duration, pressure. Effects were evaluated by a complete biomass characterization before and after treatment, with main focus on phenolic acids release. In the tested conditions and when compared to the high NaOH consumption reference extraction method for phenolic acids, the atmospheric pressure (open vessel) microwave treatment did not allow attaining high acid yields (Fig.1). The most important parameters for improving treatment efficiency were power density and solvent. In order to increase yields, microwave treatments under pressure were carried out to reach higher temperatures while taking care as to not exceed the acid denaturation temperature (150°C) and to avoid the formation of inhibitors. Phenolic acids yields and biomass composition are currently being processed and will be discussed.