Synthesis and characterization of new alkoxide and aryloxide deriavatives of titanum and zirconium. X-ray molecular structure
| Autor: | T. Cuenca, N.C. Burton, Pascual Royo, Pilar Gómez-Sal, J.I. Amor |
|---|---|
| Rok vydání: | 1995 |
| Předmět: |
Chemistry
Organic Chemistry Inorganic chemistry chemistry.chemical_element Biochemistry Medicinal chemistry Toluene Inorganic Chemistry Hexane chemistry.chemical_compound Aniline Cyclopentadienyl complex X-ray crystallography Alkoxide Materials Chemistry Lithium Physical and Theoretical Chemistry Derivative (chemistry) |
| Zdroj: | Journal of Organometallic Chemistry. 485:153-160 |
| ISSN: | 0022-328X |
| DOI: | 10.1016/0022-328x(94)05004-u |
| Popis: | Lithium or sodium alkoxides MOR (R = CHzCH=CMez; M = Li 1; Na 2; R = C6F5; M = Li 3) were prepared by reaction of the alcohols with n-butyl lithium or sodium metal in hexane. Reaction of a hexane suspension of 3 with SiCIMe 3 afforded SiMe3(OC6F 5) 4, whereas the reaction of 3 equivalents of C6FsOH with AIMe 3 in hexane led to AI(OC6Fs) 3 5. Compounds 1 or 2 react with one equivalent of [TiCp*CI2Me] (Cp* = CsMe s) in toluene to give [TiCp*C1Me(OCH2CH=CMe2)] 6. Complex 6 reacts with AIEtCI 2 to give quantitatively [TiCp*CI3]. In the presence of water, the hydrolysis of Ii takes place giving the/,-oxo compound [{(TiCp*CI)(~- O)}3]. [TiCp*CI2Me] reacted with an excess of the alcohol C6FsOH to give [TiCp*(OC6Fs) 3] 7. [ZrCpzCI 2] reacted with two equivalents of pentaflurophenol in the presence of aniline to give the dialkoxide [ZrCpz(OC6Fs)2] 8. When the same reaction was carried out in a 1 : 1 molar ratio, a mixture of 8 and the chloroalkoxide [ZrCpeCI(OC6Fs)] 9 was obtained. A clean reaction takes place when the ~-oxo compound [(ZrCp2Me)z(/x-O)] is treated with two equivalents of pentafluorophenol, leading to the isolation of the alkoxo complex [{ZrfP2(Of6Fs)}2 (/.t-O)] 10. The methylalkoxo derivative [ZrCpzMe(OC6Fs)] 11, was obtained by reaction of [ZrCpzCIMe] with one equivalent of 3. Alternative methods can also be followed to synthesize 8 and 11. The crystal and molecular structure of 8 has been determined by X-ray diffraction methods. The most interesting feature of this structure is the disposition of the (C6F 5) ring planes, which are located practically on the reflection plane defined by O(1), Zr(1) and O(1)'. |
| Databáze: | OpenAIRE |
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