Science of Synthesis

Mikami, K.; Matsumoto, Y.; Shiono, T., Science of Synthesis, (2003) 2, 493.

Trichloro(η5-cyclopentadienyl)titanium(IV) (‌79‌) can be synthesized by halogenation of dichlorobis(η5-cyclopentadienyl)titanium(IV) (‌78‌) (‌Scheme 37‌).[‌176‌] Mixed-halide complex [TiBrCpCl2] can also be obtained by this method, but [TiBr3Cp] and [TiCpI3] are only obtained in low yield. Trichloro(η5-tetrahydroindenyl)titanium(IV) (‌77‌, R1 = R2 = H) is also obtained by chlorination of dichlorobis(η5-tetrahydroindenyl)titanium(IV) in carbon tetrachlo­ride.[‌177‌] Refluxing the (2-methoxyethyl)-substituted titanium sandwich complex ‌80‌ in thio­nyl chloride/sulfuryl chloride gives the orange compound ‌81‌, whose crystal structure shows the coordination of the ether side chain to the metal center.[‌178‌] The tetrahydrofu­ran-substituted titanium–cyclopentadienyl complex ‌21‌ is obtained similarly.[‌179‌] Samuel has reported the IR and Raman spectra of tribromo(η5-cyclopentadienyl)titanium(IV), which is synthesized by addition of bromine to an ethereal solution of (η5-cyclopenta­dienyl)trimethyltitanium(IV) prepared in situ.[‌180‌]

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