R NHCOCH 3 COOH H 2 R NHCOCH 3 COOH chiral Rh catalyst * TETRAHEDRON: ASYMMETRY Tetrahedron: Asymmetry 12 (2001) 2337–2342 Pergamon A comparison of the asymmetric hydrogenation catalyzed by rhodium complexes containing chiral ligands with a binaphthyl unit and those with a 5,5,6,6,7,7,8,8-octahydro-binaphthyl unit Fu-Yao Zhang, Wai Him Kwok and Albert S. C. Chan* Open Laboratory of Chirotechnology and Department of Applied Biology and Chemical Technology, The Hong Kong Polytechnic University, Hong Kong, China Received 9 August 2001; accepted 11 September 2001 Abstract—The chiral ligands H 8 –BINAPO and H 8 –BDPAB were synthesized by reacting chlorodiphenylphosphine with H 8 BINOL and H 8 –BINAM, respectively. Applications of these ligands in the Rh-catalyzed enantioselective hydrogenation of a variety of (Z )-acetamido-3-arylacrylic acid methyl esters provided chiral amino acid derivatives with good to excellent enantiose- lectivities (H 8 –BINAPO: up to 84.0% e.e.; H 8 –BDPAB: up to 97.1% e.e.). In the hydrogenation of acetamidoacrylic acid, 99% e.e. was obtained when a [Rh(H 8 –BDPAB)] + catalyst was used. The catalytic activities and enantioselectivities of [Rh(H 8 –BINAPO)] + and [Rh(H 8 –BDPAB)] + are substantially better than those obtained with the corresponding rhodium catalysts containing BINAPO (up to 64% e.e.) and BDPAB (up to 92.6% e.e.). © 2001 Published by Elsevier Science Ltd. 1. Introduction Asymmetric catalytic hydrogenation is one of the most efficient and convenient methods for preparing a wide range of enantiomerically pure compounds. Histori- cally, the desire for practical routes to -amino acids ultimately led to the development of effective chiral diphosphine ligands, such as DIPAMP, 1 DIOP, 2 Chi- raphos, 3 Norphos, 4 BPPM, 5 BDPP, 6 BINAP, 7 Duphos, 8 BICP, 9 and others, 10 for the enantioselective hydrogenation of -amidoacrylates (-enamides) (Eq. (1)). (1) The design of such diphosphine ligands remains an active area of research, and the homogeneous asymmet- ric catalytic hydrogenation of prochiral C=X (X=C, N, O, and so forth) double bonds is one of the most important applications of these enantioselective cata- lytic reactions. It has been found that many ligands with C 2 symmetry were effective in asymmetric hydro- genation reactions. For example, the aromatic BINAP ligand, which possesses C 2 axial chirality, has shown great asymmetric induction potential. It has been sug- gested that the highly skewed position of the naphthyl rings in BINAP is the determining factor in its effective- ness in asymmetric catalytic reactions. 11 Takaya first prepared the atropisomeric ligand, H 8 BINAP, 12 which possesses a unique structural feature compared to the binaphthyl unit in BINAP. Recent research showed that the chiral catalysts derived from 5,5,6,6,7,7,8,8-octahydro-1,1-bi-2-naphthyl ligands (e.g. H 8 –BINAP, 13–15 H 8 –BINOL, 16–18 H 8 –BINAM, 18 H 8 –BDPAB, 19 H 8 –binaphthoxy, 20 H 8 –MAPs 21 ) exhibit higher efficiency and enantioselectivity for asymmetric reactions than those prepared from their parent ligands, due to the steric and electronic modulation in the H 8 –binaphthyl backbone. To expand the scope of the previous studies and to provide more support of the rationale, it is of interest to examine the effectiveness of chiral ligands H 8 –BINAPO 1 and H 8 –BDPAB 3 in comparison with BINAPO 2 and BDPAB 4 in the asymmetric hydrogenation of dehydroamino acid derivatives and other substrates. Herein, we report the results of this comparative study and provide more evidence for the superior properties of the partially hydrogenated binaphthyl species (Fig. 1). * Corresponding author. Fax: 852-23649932; e-mail: bcachan@ polyu.edu.hk 0957-4166/01/$ - see front matter © 2001 Published by Elsevier Science Ltd. PII:S0957-4166(01)00399-8