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We developed a hydrodehalogenation reaction of polyhaloalkanes catalyzed by paddlewheel dimolybdenum complexes in combination with 1-methyl-3,6-bis(trimethylsilyl)-1,4-cyclohexadiene (MBTCD) as a non-toxic H-atom source as well as a salt-free reductant. A mixed-ligated dimolybdenum complex Mo 2 (OAc) 2 [CH(NAr) 2 ] 2 ( 3a , Ar = 4-MeOC 6 H 4 ) having two acetates and two amidinates exhibited high catalytic activity in the presence of  n  Bu 4 NCl, in which [  n  Bu 4 N] 2 [Mo 2 {CH(NAr) 2 } 2 Cl 4 ] ( 9a ), derived by treating 3a with ClSiMe 3 and  n  Bu 4 NCl, was generated as a catalytically-active species in the hydrodehalogenation. All reaction processes, oxidation and reduction of the dimolybdenum complex, were clarified by control experiments, and the oxidized product, [  n  Bu 4 N][Mo 2 {CH(NAr) 2 } 2 Cl 4 ] ( 10a ), was characterized by EPR and X-ray diffraction studies. Kinetic analysis of the hydrodehalogenation reaction as well as a deuterium-labelling experiment using MBTCD- d  8 suggested that the H-abstraction was the rate-determining step for the catalytic reaction.

Mixed-ligand complexes of paddlewheel dinuclear molybdenum as hydrodehalogenation catalysts for polyhaloalkanes