1,1,3,3-Tetramethylguanidine solvated lanthanide aryloxides: pre-catalysts for intramolecular hydroalkoxylation.
In: Dalton transactions (Cambridge, England : 2003), 2009-12-21, Heft 47, S. 10601-8
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Zugriff:
The synthesis and structural characterization of six 1,1,3,3-tetramethylguanidine (H-TMG) solvated lanthanide aryloxide complexes are reported. Ln[N{Si(CH3)3}2]3 (Ln = Nd, La) was reacted with two equivalents of both H-TMG and HOAr {HOAr = HOC6H2(CMe3)2-2,6 (H-DBP) or HOC6H2(CMe3)2-2,6-CH3-4 (H-4MeDBP)} and one equivelent of ethanol (HOEt) to yield the corresponding [Nd(H-TMG)2(4MeDBP)2(OEt)] (1) and [La(H-TMG)2(DBP)2(OEt)] (2). Compounds 1 and 2 were further reacted with 4-pentyn-1-ol {HO(CH2)3C[triple bond]CH} to isolate [Nd(H-TMG)2(4MeDBP)2{O(CH2)3C[triple bond]CH}] (3) and [La(H-TMG)2(DBP)2{O(CH2)3C[triple bond]CH}] (4), respectively. Three equivalents of HOAr and one equivalent of H-TMG were additionally reacted with Ln[N{Si(CH3)3}2]3 to generate [Nd(4MeDBP)3(H-TMG)] (5) and [La(DBP)3(H-TMG)] (6). In order to examine the formation of 1-6, the interaction of H-TMG and HOAr was further examined in solution and the hydrogen bonded complexes (H-TMG:HOAr), 7 and 8, were isolated. Upon successful isolation of 1-6, the utility of 1, 2, 4 and 5 as pre-catalysts for the intramolecular hydroalkoxylation of 4-pentyn-1-ol was investigated. The bulk powders for all complexes were found to be in agreement with the crystal structures based on elemental analyses, FT-IR spectroscopy, and 1H and 13C NMR investigations.
Titel: |
1,1,3,3-Tetramethylguanidine solvated lanthanide aryloxides: pre-catalysts for intramolecular hydroalkoxylation.
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Autor/in / Beteiligte Person: | Janini, TE ; Rakosi R 3rd ; Durr, CB ; Bertke, JA ; Bunge, SD |
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Zeitschrift: | Dalton transactions (Cambridge, England : 2003), 2009-12-21, Heft 47, S. 10601-8 |
Veröffentlichung: | Cambridge, UK : Royal Society of Chemistry, c2003-, 2009 |
Medientyp: | academicJournal |
ISSN: | 1477-9234 (electronic) |
DOI: | 10.1039/b917377c |
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