Layered double hydroxides (LDHs) or hydrotalcite-like materials of the type Mg1 -xAlx(OH) 2 (Xn- ) x/n ·zH2O are most readily prepared when Xn- is the carbonate ion. Although many other LDHs undergo facile ion-exchange reactions, the carbonate ion in LDHs is known to be very difficult to replace by conventional ion-exchange. We have developed a simple synthesis of adipate-pillared LDHs of the type Mg4A12 (OH) 12 [O2C (CH2)4CO2]· 4H2O by direct reaction of free adipic acid with an LDH carbonate precursor. The materials obtained have been characterized by XRD, FT-IR and DTA. It is shown that by appropriate choice of reaction conditions, the carbonate ions in the precursor can be completely replaced by adipate ions. The adipate-pillared LDHs retain a layered structure with an interlayer distance of 1. 40urn. The interlayer adipate ions are lost on heating the material to 39℃.