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Functionalised tris(pyrazolyl)methane ligands and Re(CO)3 complexes thereof


Kunz, P C; Berghahn, M; Brückmann, N E; Dickmeis, M; Kettel, M; Spingler, B (2009). Functionalised tris(pyrazolyl)methane ligands and Re(CO)3 complexes thereof. Zeitschrift für Anorganische und Allgemeine Chemie, 35(3):471-478.

Abstract

The synthesis of new tripodal nitrogen ligands derived from tris(pyrazolyl)methane (TpmR, R = H, tBu, Ph in 3-position) is described. After deprotonation of the parent tris(pyrazolyl)methane TpmR, the carbanion reacts readily with ethylene oxide to yield the 3,3,3-tris(3-substituted pyrazolyl)propanol ligands[(3-Rpz)3CCH2CH2OH, R = H, tBu, Ph, 1a-c]. These ligands can be easily derivatised at the alcohol function. Microwave-assisted reactions of these ligands and [Re(CO)5Br] yields the complex [(1a)Re(CO)3]Br (4) in the case of ligand 1a, whereas in the case of the substituted ligands 1b and 1c degradation was observed. The degradation products are identified as [(HpzR)2Re(CO)3Br] [R = tBu (7b), Ph (7c)]. These complexes were also prepared directly from [Re(CO)5Br] and the corresponding pyrazoles by microwave-assisted synthesis. The Re(CO)3 complexes 4 and [(1a)Re(CO)3]OTf (5) are water-soluble. The structures of 5·H2O and [{(pz)3CCH2CH3}Re(CO)3]OTf·1.5H2O·1/2CH3CN (6·1.5H2O·1/2CH3CN) as well as the structure of 7b have been elucidated by X-ray crystallography.

The synthesis of new tripodal nitrogen ligands derived from tris(pyrazolyl)methane (TpmR, R = H, tBu, Ph in 3-position) is described. After deprotonation of the parent tris(pyrazolyl)methane TpmR, the carbanion reacts readily with ethylene oxide to yield the 3,3,3-tris(3-substituted pyrazolyl)propanol ligands[(3-Rpz)3CCH2CH2OH, R = H, tBu, Ph, 1a-c]. These ligands can be easily derivatised at the alcohol function. Microwave-assisted reactions of these ligands and [Re(CO)5Br] yields the complex [(1a)Re(CO)3]Br (4) in the case of ligand 1a, whereas in the case of the substituted ligands 1b and 1c degradation was observed. The degradation products are identified as [(HpzR)2Re(CO)3Br] [R = tBu (7b), Ph (7c)]. These complexes were also prepared directly from [Re(CO)5Br] and the corresponding pyrazoles by microwave-assisted synthesis. The Re(CO)3 complexes 4 and [(1a)Re(CO)3]OTf (5) are water-soluble. The structures of 5·H2O and [{(pz)3CCH2CH3}Re(CO)3]OTf·1.5H2O·1/2CH3CN (6·1.5H2O·1/2CH3CN) as well as the structure of 7b have been elucidated by X-ray crystallography.

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Additional indexing

Item Type:Journal Article, refereed, original work
Communities & Collections:07 Faculty of Science > Department of Chemistry
Dewey Decimal Classification:540 Chemistry
Language:English
Date:2009
Deposited On:06 Feb 2010 10:11
Last Modified:05 Apr 2016 13:52
Publisher:Wiley-Blackwell
ISSN:0044-2313
Additional Information:Published in: Zeitschrift für anorganische und allgemeine Chemie. Volume 635 Issue 3, 2009
Publisher DOI:10.1002/zaac.200801298
Permanent URL: http://doi.org/10.5167/uzh-29590

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