Applied Catalysis A: General 262 (2004) 43–51 On the catalytic properties of mixed oxides obtained from the Cu-Mg-Al LDH precursors in the process of hydrogenation of the cinnamaldehyde J. Barrault a, , A. Derouault a , G. Courtois a , J.M. Maissant a , J.C. Dupin b , C. Guimon b , H. Martinez b , E. Dumitriu c a Laboratoire de Catalyse en Chimie Organique (LACCO), UMR CNRS 6503, ESIP, 40 Avenue du Recteur Pineau, 86022 Poitiers Cedex, France b LPCM, UMR 5624, 2 Avenue P. Angot, 64053 Pau Cedex9, France c Laboratory of Catalysis, Technical University of Iasi, Iasi, Romania Received in revised form 3 November 2003; accepted 12 November 2003 Abstract Catalytic hydrogenation of cinnamaldehyde (CNA) was investigated over oxidic materials obtained by the calcination of Cu-Mg-Al layered double hydroxide (LDH) precursors. A series of precursors with different Cu/Mg ratios (with a constant M 2+ /Al 3+ ratio) were prepared by coprecipitation (under low supersaturation) and heated under reductive atmosphere until 623K in order to avoid the formation of Cu-based spinels and to reduce the copper cations. The presence of Mg noticeably enhanced the selectivity of Cu-based catalysts with respect to the hydrogenation of the carbonyl group relative to the favoured hydrogenation of the C=C bond. Moreover, the self-condensation of hydrocinnamaldehyde (HCNA) and the cross-condensation of hydrocinnamaldehyde with cinnamaldehyde were also observed especially when the basic sites of LDH structures are preponderant over hydrogenation species. Finally, all that reaction from CNA are of great interest for getting information about: (i) basic sites involved in condensation of CNA and HCNA; and (ii) active species for selective hydrogenation of CNA to cinnamyl alcohol (CNOL) which seem in strong interaction with the first ones. © 2003 Elsevier B.V. All rights reserved. Keywords: Hydrogenation; Cinnamaldehyde; Layered double hydroxides; Mixed oxides; Aldol condensation 1. Introduction The chemio- and regioselective catalytic hydrogenation of ,-unsaturated aldehydes, such as cinnamaldehyde, is of great importance in the synthesis of valuable fine chem- icals. Both the cinnamaldehyde and the cinnamyl alcohol (CNOL), the last being obtained by the selective reduction of the cinnamaldehyde, are widely used in perfumes and flavouring industries. In addition, cinnamyl alcohol is an im- portant building block in organic synthesis. Normally, dur- ing the hydrogenation of cinnamaldehyde (CNA), both the carbonyl C=O group and the C=C double bond are hydro- genated to hydrocinnamaldehyde (HCNA) and CNOL via two parallel processes (1) and (2) in Scheme 1, and finally to hydrocinnamyl alcohol (HCNOL). Corresponding author. Tel.: +33-549-453999; fax: +33-549-453349. E-mail address: joel.barrault@univ-poitiers.fr (J. Barrault). Although hydrogenation of the C=C bond is thermody- namically more favourable, numerous studies were done to enhance the selective hydrogenation of the C=O bond. The most successful attempts were carried out in the presence of heterogeneous catalysts prepared from metals belonging to group VIII, such as Pt, Ir, Os, etc. It was observed that the reaction selectivity is influenced by several parameters such as the metal particle size, the precursor, the method of preparation, the support (Al 2 O 3 [1], SiO 2 [2], zeolite [3,4], clays [5], carbon nanofibres [6,7], etc.), the nature of the solvent [8] or the application of the ultrasonic irradiation [9]. Often, the selectivity to the unsaturated alcohol required catalyst modification and promotion, such as the addition of transition metal salts, promoters (e.g. Ge, Sn, Pb [10,11]) or alloying the base metal of the catalyst with another one [12]. Besides the noble metal-based catalysts, other catalytic materials, such as those containing Cu, were investigated for 0926-860X/$ – see front matter © 2003 Elsevier B.V. All rights reserved. doi:10.1016/j.apcata.2003.11.020