Elsevier, Polyhedron, 26-27(20), p. 3225-3229
DOI: 10.1016/s0277-5387(01)00931-7
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The reaction between benzyl-benzylidene-amine (1) and Pd(OAc)(2) in acetic acid has been reexamined in order to prepare its acetato bridged endo-cyclopalladated dimer, (mu -OAc)(2)[Pd(C6H4CH=NCH2C6H5)](2) (2), in high yield. The best results were obtained when 1 and Pd(OAc)(2) in a molar ratio of 2:1 were treated under reflux in acetic acid for 45 min. Under these conditions, 2 was isolated in 85% yield. Further, 2 reacted with LiCl, giving the corresponding chloro bridged cyclopalladated dimer (mu -Cl)(2)[Pd(C6H4CH=NCH2C6H5)](2) (3), which was isolated in 80% yield. In addition, 2 and 3 were converted into the mononuclear cyclopalladated compounds trans-N,P-[Pd(C6H4CH=NCH2C6H5)(OAc)(PPh3)] (4), trans -N,P-[Pd(C6H4CH=NCH2C6H5)-(Cl)(PPh3)] (5) and [Pd(C6H4CH=NCH2C6H5)(acac)] (6), which were characterised by elemental analysis, FAB(+), IR and NMR spectra. The reactivity of 4 and 5 towards solutions of PPh3 in CDCl3 showed that PPh3 was not a good enough sigma donor ligand to cleave the sigma (Pd-N) of 4 and 5.