1206101-01-0Relevant articles and documents
1,1,3,3-Tetramethylguanidine solvated lanthanide aryloxides: Pre-catalysts for intramolecular hydroalkoxylation
Janini, Thomas E.,Rakosi III, Robert,Durr, Christopher B.,Bertke, Jeffrey A.,Bunge, Scott D.
, p. 10601 - 10608 (2009)
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 = HOC 6H2(CMe3)2-2,6 (H-DBP) or HOC 6H2(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)3CCH} to isolate [Nd(H-TMG)2(4MeDBP)2{O(CH2)3CCH}] (3) and [La(H-TMG)2(DBP)2{O(CH2) 3CCH}] (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.
