The assembly of biorgano-guest to laminar inorganic solids is of increasing interest to their versatile applications in biotechnology or catalysis. We synthesized two different biohybrid materials based on L-leu into the hydrotalcite rehydrated under ultrasound treatment (HT(rus)), in which L-leu was immobilized by intercalation or by replacing of hydroxyl ions at the edge sites of HT(rus). Separately L-leu and HT(rus) as catalysts showed very poor activity and lack of enantioselectivity in the epoxidation reaction of alpha,beta-unsaturated ketones such as chalcone. Nevertheless, the catalysts presented high activity and even enantioselectivity towards the trans-(R,S)-epoxide depending on the L-leu location on the nanohybrid catalyst. (C) 2011 Elsevier B.V. All rights reserved.