Liquid-phase separations of similarly sized organic molecules using membranes is a major challenge for energy-intensive industrial separation processes. We created free-standing carbon molecular sieve membranes that translate the advantages of reverse osmosis for aqueous separations to the separation of organic liquids. Polymer precursors were cross-linked with a one-pot technique that protected the porous morphology of the membranes from thermally induced structural rearrangement during carbonization. Permeation studies using benzene derivatives whose kinetic diameters differ by less than an angstrom show kinetically selective organic liquid reverse osmosis. Ratios of single-component fluxes forpara- andortho-xylene exceeding 25 were observed andpara- andortho- liquid mixtures were efficiently separated, with an equimolar feed enriched to 81 mole %para-xylene, without phase change and at ambient temperature.