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• W2092307277 abstract "The mixed chloro-aryloxide compounds of stoichiometry M(OAr-2,6Ph2)2Cl3 and [M(OAr-2,6Ph2)3Cl2] (M = Nb, Ta; OAr-2,6Ph2 = 2,6-diphenylphenoxide) serve as useful substrates for the synthesis of a series of corresponding tris- and bis-alkyl derivatives. Thermolysis of these alkyl compounds in hydrocarbon solvents leads to the formation of cyclometallated compounds of the type M(OC6H3Ph-C6H4)(OAr-2,6Ph2)(R)2 and M(OC6H3Ph-C6H4)(OAr-2,6Ph2)2(R) (R = CH3, CH2-C6H4-4Me). Reduction of the dichlorides M(OAr-2,6Ph2)3Cl2 with sodium amalgam in toluene solution does not yield the corresponding tris-aryloxides. Instead the bis-cyclometallated compounds M(OC6H3Ph-C6H4)2(OAr-2,6Ph2) (M = Nb, Ta) are produced in high yield along with H2. However, in the presence of one atmosphere of H2 the niobium compound undergoes reduction to produce Nb(OC6H3Ph-η4-C6H7)(OAr-2,6Ph2)2. Spectroscopic and structural studies of this latter compound show it to contain an η4-bound cyclohexadiene ring formed by hydrogenation of an ortho-phenyl substituent of an aryloxide ligand. Treatment of the niobium cyclohexadiene complex with H2 (1000 psi, 25°C) leads to the hydrogenation of the original 2,6-diphenylphenoxide ligands to produce, after hydrolysis, high yields of 2,6-dicyclohexylphenol. The selective side chain hydrogenation of 2,6-diphenylphoxide ligands can also be achieved by reacting alkyl compounds such as Nb(OAr-2,6Ph2)3Me2 with H2. In this latter case a mono-hydride of stoichiometry Nb(H)(OAr-2,6cy2)4 was isolated and structurally characterized." @default.
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• W2092307277 date "1989-01-01" @default.
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• W2092307277 title "The metallation and hydrogenation of aryl rings in early transition metal aryloxide systems" @default.
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• W2092307277 doi "https://doi.org/10.1016/s0277-5387(00)80604-x" @default.
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