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Synthesis of an (/eta//sup 3/-allyl(hydrido)iridium complex and its reactions with arenes and alkanes. Sequential intermolecular C-H oxidative addition and hydride-to-alkene migratory insertion reactions

Journal Article · · J. Am. Chem. Soc.; (United States)
DOI:https://doi.org/10.1021/ja00221a026· OSTI ID:5993226

The iridium allyl hydride complex (/eta//sup 5/-C/sub 5/Me/sub 5/)(/eta//sup 3/-C/sub 3/H/sub 5/)(H)Ir (2) has been prepared from ((/eta//sup 5/-C/sub 5/Me/sub 5/)IrCl/sub 2/)/sub 2/, and its reaction with arenes and alkanes has been investigated. The hydride reacts with C-H bonds in benzene and cyclopropane in the presence of phosphines L, leading to the phenyl and cyclopropyl complexes (/eta//sup 5/-C/sub 5/Me/sub 5/)(L)Ir(n-propyl)(R) (3,4, and 5). Irradiation of 2 in the presence of PMe/sub 3/ takes a different course, giving the previously uncharacterized (/eta//sup 5/-C/sub 5/Me/sub 5/)Ir(PMe/sub 3/)/sub 2/ (6). Thermal reaction of 2 in alkane solvents such as n-butane and isobutane, which are capable of ..beta..-elimination, leads to products 8a, 8b, and 9 formed by replacement of the allyl group in 2 by a substituted allyl ligand formed by overall dehydrogenation of the alkane. Thermolysis of 2 in the presence of arenes such as n-propylbenzene and cumene leads to more complicated products resulting from intermolecular C-H activation followed by cyclometalation (e.g., 13, 15) and/or dimerization (20). The structure of cyclometalated dimer 20 has been determined by X-ray diffraction. Mechanistic studies, including kinetics, isotope tracer experiments, and intra-versus intermolecular isotope effect determinations, implicate the coordinatively unsaturated species (/eta//sup 5/-C/sub 5/Me/sub 5/)(/eta//sup 2/-propene)Ir (complex A in Scheme XX) as the initially formed intermediate in the thermal reactions of 1 with alkanes and arenes. Significant differences exist between the behavior of this intermediate (cf. Schemes XIX and XXIII) and that of the closely related phosphine-substituted complex (/eta//sup 5/-C/sub 5/Me/sub 5/)(PMe/sub 3/Ir) studied earlier; possible reasons for these differences are discussed.

Research Organization:
Lawrence Berkeley Lab., CA (USA)
DOE Contract Number:
AC03-76SF00098
OSTI ID:
5993226
Journal Information:
J. Am. Chem. Soc.; (United States), Journal Name: J. Am. Chem. Soc.; (United States) Vol. 110:13; ISSN JACSA
Country of Publication:
United States
Language:
English