Abstract
Pinacolone- N, N-dimethylhydrazone was regiospecifically cyclopalladated by Pd(OAc) 2 in glacial acetic acid on the C(Me)N-methyl group to give the acetato-bridged complex [Pd{CH 2C(CMe 3)NNMe 2}(μ-O 2CMe)] 2 ( 1). Subsequent treatment with aqueous sodium chloride or bromide gave the corresponding halide-bridged complexes [Pd{CH 2C(CMe 3)NNMe 2}(μ-X)] 2 ( 2, X=Cl; 3, X=Br). Treatment of 2 and 3 with tertiary diphosphines in a 1:1 molar ratio yielded the dinuclear complexes [{Pd[CH 2C(CMe 3)NNMe 2](X)} 2{μ-Ph 2PRPPh 2}] ( 4, 5, R=CH 2; 6, 7, R=CHMe; 8, 9, R=CCH 2; 10, 11, R=NMe; 12, 13, R= trans-CHCH, 14, 15, R=C 2H 4, 16, 17, R=C 3H 6; 18, 19, R=C 4H 8). Treatment of 2 and 3 with AgClO 4 and the appropriate diphosphine ligand in a 1:2 molar ratio, afforded the mononuclear species [Pd{CH 2C(CMe 3)NNMe 2}(Ph 2PRPPh 2- P, P′)][ClO 4]}] ( 20, R=CH 2; 21, R=CHMe; 22, R=CCH 2; 23, R=NMe; 24, R= cis-CHCH, 25, R=C 2H 4, 26, R=C 3H 6; 27, R=C 4H 8). The complexes were characterized by elemental analysis (C, H, N), conductivity measurements, IR and 1H and 31P{ 1H} NMR spectroscopy, and by mass spectrometry.
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