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2.10.5.2 Method 2: Titanium(III) Complexes by Reduction of Titanium(IV) Complexes by Lithium Nitride

DOI: 10.1055/sos-SD-002-00576

Mikami, K.; Matsumoto, Y.; Shiono, T.Science of Synthesis, (20032502.

In coordinating solvents, lithium nitride acts as a reducing reagent, liberating dinitrogen; for example, titanium(IV) chloride is reduced by lithium nitride to Li[TiCl4]4THF, [Ti(Cp)2Cl2] (78) is reduced to [{Ti(Cp)2Cl}2] (92), and [TiCpCl3] (79) is reduced to [TiCpCl2(THF)] (93) (Scheme 44).[‌213‌] This preparative method has distinct advantages over the standard method which uses zinc dust as the reductant, in that it avoids the formation of the bis[chlorobis(η5-cyclopentadienyl)titanium(III)]zinc(II) chloride complex, [{Ti(Cp)2Cl}2]ZnCl2, which is often a major product. The method has advantages over the reaction between dichlorobis(η5-cyclopentadienyl)titanium(IV) (78) and [Ti(BH4)(Cp)2], since it avoids the prior preparation of the latter complex.

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References


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