A novel route to heterogenize an organorhenium(VII) oxide, derived from the well examined methyltrioxorhenium(VII) (MTO), on the surface of an iodosilane-modified MCM-41 is applied. The successful grafting of the -CH(2)-ReO3 moiety on the surface was evidenced by 1H CP MAS NMR, IR spectroscopy, TG-MS, and elemental analysis. XRD and TEM analyses confirm the retaining of long-range ordering throughout the grafting process. The rhenium loading of the mesoporous material after heterogenization of MTO is found to be 1.25 wt%. Despite containing formally a derivative of the very sensitive benzyltrioxorhenium(VII) the material is stable at room temperature and applicable as a heterogeneous catalyst for aldehyde olefination reactions.
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Synthesis, characterization and application of organorhenium(vii) trioxides in metathesis reactions and epoxidation catalysis.
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Molecular Catalysis, Catalysis Research Center and Department of Chemistry, Technische Universität München, Lichtenbergstr. 4, 85747 Garching bei München, Germany.
Four novel organorhenium(vii) oxides of the type L-ReO3 are presented: [4-(trifluoromethyl)phenyl]trioxorhenium 1b, [4-(trifluoromethoxy)phenyl]trioxorhenium 2b, [4-(trifluoromethyl)tetrafluorophenyl]trioxorhenium(THF) 3b·THF and (2,2,6,6-tetramethylpiperidin-1-yl)trioxorhenium 5. As intermediate products, the novel diarylzinc compounds bis[4-(trifluoromethoxy)phenyl]zinc 2a and bis[2,6-bis(trifluoromethyl)phenyl]zinc 4a were prepared. The properties and structure of 1b-5 were studied by means of 1H, 13C, 19F and 17O NMR, IR, MS, TGA and elemental analysis.
View Article and Find Full Text PDFHeterogenization of an organorhenium(VII) oxide on a modified mesoporous molecular sieve.
Dalton Trans
January 2006
Lehrstuhl für Anorganische Chemie der Technischen Universität München, Lichtenbergstrasse 4, D-85747, Garching bei München, Germany.
A novel route to heterogenize an organorhenium(VII) oxide, derived from the well examined methyltrioxorhenium(VII) (MTO), on the surface of an iodosilane-modified MCM-41 is applied. The successful grafting of the -CH(2)-ReO3 moiety on the surface was evidenced by 1H CP MAS NMR, IR spectroscopy, TG-MS, and elemental analysis. XRD and TEM analyses confirm the retaining of long-range ordering throughout the grafting process.
View Article and Find Full Text PDFOrganorhenium(VII) and organomolybdenum(VI) oxides: syntheses and application in olefin epoxidation.
Dalton Trans
August 2005
Lehrstuhl für Anorganische Chemie der Technischen Universität München, Lichtenbergstrasse 4, D-85747, Garching bei München, Germany.
The first members of the classes of the organorhenium(VII) oxides and organomolybdenum(VI) oxides were described during the 1960s and 1970s. However, despite the fact that methyltrioxorhenium(VII)(MTO) is probably the best examined organometallic oxide known, many of its derivatives as well as the Mo congeners were not tested for any application. Nevertheless, it is known that several organomolybdenum oxides, particularly those of formula eta5-(C5R5)MoO2Cl and eta5-(C5R5)MoO2R' are powerful epoxidation catalysts if applied together with tert-butylhydroperoxide (TBHP).
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