Please use this identifier to cite or link to this item: http://hdl.handle.net/10773/19820
Title: Synthesis and characterization of CpMo(CO)(3)(CH2-pC(6)H(4)-CO2CH3) and its inclusion compounds with methylated cyclodextrins. Applications in olefin epoxidation catalysis
Author: Gomes, Ana C.
Bruno, Sofia M.
Tome, Catia
Valente, Anabela A.
Pillinger, Martyn
Abrantes, Marta
Goncalves, Isabel S.
Keywords: CYCLOPENTADIENYL-MOLYBDENUM COMPLEXES
TUNGSTEN COMPLEXES
ETA(5)-CYCLOPENTADIENYL MOLYBDENUM
MESOPOROUS MATERIALS
TRICARBONYL COMPLEX
CYCLOALKYL MOIETIES
CARBONYL-COMPLEXES
BETA-CYCLODEXTRIN
BRIDGING UNITS
ANSA COMPOUNDS
Issue Date: 2013
Publisher: ELSEVIER SCIENCE SA
Abstract: The cyclopentadienyl molybdenum tricarbonyl complex CpMo(CO)(3)(CH2-pC(6)H(4)-CO2CH3) (1) (Cp = eta(5)-C5H5) and its 1:1 inclusion complexes with heptakis(2,6-di-O-methyl)-beta-cyclodextrin (1@DIMEB) and heptakis(2,3,6-tri-O-methyl)-beta-cyclodextrin (1@TRIMEB) were prepared and characterized by elemental and thermogravimetric analyses, powder X-ray diffraction, NMR, FT-IR and Raman spectroscopy. All three compounds were investigated as catalyst precursors for olefin epoxidation using cis-cyclooctene (Cy) as a model substrate, a reaction temperature of 55 degrees C, and different types of oxidants (tert-butylhydroperoxide in decane;(TBHPdec) or in water (TBHPaq), and aqueous hydrogen peroxide). With the aim of facilitating recycling of the homogeneous catalytic systems, different solvent mixtures were tested: biphasic liquid-liquid solvent systems [(water, glycerol, ionic liquid)-(n-hexane, alpha,alpha,alpha-trifluorotoluene (TFT), iso-butyl methyl ketone)], and in some cases no cosolvent was added. Excellent epoxide selectivity (100%) was observed for all tested catalytic systems. An example of an interesting catalytic system is that of 1@TRIMEB/TBHPaq/TFT/H2O since the catalyst can be easily separated in the form of an aqueous solution, by decantation, from the organic phase containing the reaction products and recycled. (C) 2013 Elsevier B.V. All rights reserved.
Peer review: yes
URI: http://hdl.handle.net/10773/19820
DOI: 10.1016/j.jorganchem.2012.12.019
ISSN: 0022-328X
Publisher Version: 10.1016/j.jorganchem.2012.12.019
Appears in Collections:CICECO - Artigos



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