Green efficient organocatalytic heterogeneous epoxidation of trans-methylcinnamate was achieved on LDH-intercalated levulinate using H2O2/acetonitrile as oxidant. The layered double hydroxide (LDH) was prepared by co-precipitation starting from an aqueous solution of Mg(NO3)(2).6H(2)O and Al(NO3)(3).9H(2)O. The preparation of the LDH hybrid organocatalyst was carried out following four different routes: i) step-by-step ion exchange in air (LEV@LDH-air); ii) one charge ion-exchange in N-2 atmosphere (LEV@LDH-N-2); iii) direct synthesis by co-precipitation (LEV@LDH-pp); and the iv) reconstruction method (LEV@LDH-mem). The synthesized catalysts were characterized using different techniques such as adsorption-desorption isotherms of nitrogen at -196 degrees C, powder X-ray diffraction (XRD), differential thermal analysis and thermogravimetric analysis (TG-DTA), and diffuse reflectance infrared Fourier transform (DRIFT) spectroscopy techniques. The levulinate was successfully intercalated by ion exchange and co-precipitation. In the investigated series the LEV@LDH-pp catalyst showed the highest performances at 40 degrees C and 24 h (C-cinnamate = 21.4%, S-glycidate = 100%). (C) 2016 Elsevier B.V. All rights reserved.