AbstractPolyester copolymers were prepared with β‐cyclodextrin (β‐CD) and sebacoyl (SCl) or terephthaloyl (TCl) chloride cross linker agents using a simple, one‐pot synthesis. Variation of the mole ratios (i.e., 1 : 1, 1 : 2, 1 : 3, 1 : 6, and 1 : 9) of β‐CD to diacid chloride linker units resulted in copolymers with differing solubility and chemical stability in aqueous solution. The sorption properties of copolymers such as 1 : 6 and 1 : 9 SCl, and 1 : 9 TCl materials were investigated because of their relative insolubility and resistance to hydrolysis at pH 4.6. The monolayer sorption capacity (Qm) of the copolymers varied according to the nature of the cross linker and the relative mole ratio of monomers. Qm values obtained from the Sips isotherm model range from 2.7 to 5.2 mmol/g for the sorption of p‐nitrophenol at 295 K and approach the value of Qm for a commercially available granular activated carbon sorbent. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013