Liquid-phase exfoliation is the most suitable platform for large-scale production of two-dimensional materials. One of the main open challenges is related to the quest of green and bioderived solvents to replace state-of-the-art dispersion media, which suffer several toxicity issues. Here, we demonstrate the suitability of methyl-5-(dimethylamino)-2-methyl-5-oxopentanoate (Rhodiasolv Polarclean) for sonication-assisted liquid-phase exfoliation of layered materials for the case-study examples of WS2, MoS2, and graphene. We performed a direct comparison, in the same processing conditions, with liquid-phase exfoliation using N-methyl-2-pyrrolidone (NMP) solvent. The amount of few-layer flakes (with thickness