The aim of this study is to improve the dissolution properties of a poorly‐soluble active substance, Eflucimibe by associating it with gamma‐cyclodextrin. To achieve this objective, a new three‐step process based on supercritical fluid technology has been proposed. First, Eflucimibe and cyclodextrin are co‐crystallized using an anti‐solvent process, dimethylsulfoxide being the solvent and supercritical carbon dioxide being the anti‐solvent. Second, the co‐crystallized powder is held in a static mode under supercritical conditions for several hours. This is the maturing step. Third, in a final stripping step, supercritical CO2 is flowed through the matured powder to extract the residual solvent. The coupling of the first two steps brings about a significant synergistic effect to improve the dissolution rate of the drug. The nature of the entity obtained at the end of each step is discussed and some suggestions are made as to what happens in these operations. It is shown the co‐crystallization ensures a good dispersion of both compounds and is rather insensitive to the operating parameters tested. The maturing step allows some dissolution‐recrystallization to occur thus intensifying the intimate contact between the two compounds. Addition of water is necessary to make maturing effective as this is governed by the transfer properties of the medium. The stripping step allows extraction of the residual solvent but also removes some of the Eflucimibe which is the main drawback of this final stage.