期刊
INORGANIC CHEMISTRY
卷 52, 期 19, 页码 11126-11135出版社
AMER CHEMICAL SOC
DOI: 10.1021/ic401363p
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资金
- National Science Foundation/Department of Energy [NSF/CHE-0822838]
- U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences [DE-AC02-06CH11357]
- Chemical Sciences, Geosciences and Biosciences Division, Office of Basic Energy Science, Office of Science, U.S. Department of Energy [DE-FG02-07ER15893]
- Division Of Chemistry
- Direct For Mathematical & Physical Scien [0822838] Funding Source: National Science Foundation
The bulky aryloxide 2,6-bis(diphenylmethyl)-4-tert-butylphenol [HOArtBu] (1) can be synthesized from 4-tert-butylphenol and benzhydrol in solvent-free conditions and obtained pure in 91% yield. Deprotonation of HOArtBu is accomplished with M(N(SiMe3)(2)) (M = Na, Li), yielding the corresponding salts of the aryloxide [MOArtBu (M+ = Na (2), Li(3)) in 83% and 73% yield, respectively. Facile salt formation of the aryloxide ligand allows for transmetalation to a variety of metal halides. Through transmetalation reactions involving two aryloxides, mononuclear complexes of the type [M'(OArtBu)(2)Cl(THF)(2)] (M' = Sc (4), V (5), Cr (6), Ti (7)) can be prepared from the corresponding metal halide precursor MCl3(THF)(3). Additionally, two aryloxides can be coordinated to Ti(IV) via a protonolysis route of Ti(NMe2)(2)Cl-2 and 2 equiv of HOArtBu to yield [TKOArtBu)(2)Cl-2(NHMe2)] (8) in 72% isolated yield. Single-crystal X-ray diffraction studies of 1, 2, and the 3d metal complexes 5-8 clearly show the steric demand of the bulky ligand, whereas in transition metal complexes we do not observe the formation of mononuclear tris-aryloxide complexes.
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