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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >1,1,3,3-Tetramethylguanidine solvated lanthanide aryloxides: Pre-catalysts for intramolecular hydroalkoxylation
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1,1,3,3-Tetramethylguanidine solvated lanthanide aryloxides: Pre-catalysts for intramolecular hydroalkoxylation

机译：1,1,3,3-四甲基胍溶剂化的镧系元素芳氧化物：分子内加氢烷氧基化的前催化剂

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摘要

The synthesis and structural characterization of six 1,1,3,3- tetramethylguanidine (H-TMG) solvated lanthanide aryloxide complexes are reported. Ln[N{Si(CH_3)_3}_2]_3 (Ln = Nd, La) was reacted with two equivalents of both H-TMG and HOAr {HOAr = HOC_ 6H_2(CMe_3)_2-2,6 (H-DBP) or HOC_ 6H_2(CMe_3)_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(CH_2)_3CCH} to isolate [Nd(H-TMG)_2(4MeDBP)_2{O(CH_2)_3CCH}] (3) and [La(H-TMG)_2(DBP)_2{O(CH_2)_ 3CCH}] (4), respectively. Three equivalents of HOAr and one equivalent of H-TMG were additionally reacted with Ln[N{Si(CH_3)_ 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 ~(13)C NMR investigations.
机译：报道了六个1,1,3,3-四甲基胍（H-TMG）溶剂化的镧系元素芳氧基配合物的合成和结构表征。 Ln [N {Si（CH_3）_3} _2] _3（Ln = Nd，La）与两个当量的H-TMG和HOAr反应（HOAr = HOC-6H_2（CMe_3）_2-2,6（H-DBP）或HOC_ 6H_2（CMe_3）_2-2,6-CH3-4（H-4MeDBP）}和一当量的乙醇（HOEt），得到相应的[Nd（H-TMG）_2（4MeDBP）_2（OEt）]（ 1）和[La（H-TMG）_2（DBP）_2（OEt）]（2）。使化合物1和2与4-戊炔-1-醇{HO（CH_2）_3CCH}反应，分离出[Nd（H-TMG）_2（4MeDBP）_2 {O（CH_2）_3CCH}]（3）和[La （H-TMG）_2（DBP）_2 {O（CH_2）_ 3CCH}]（4）。使三当量的HOAr和一当量的H-TMG与Ln [N {Si（CH_3）_ 3} _2] _3反应生成[Nd（4MeDBP）_3（H-TMG）]（5）和[La （DBP）_3（H-TMG）]（6）。为了检查1-6的形成，在溶液中进一步检查了H-TMG和HOAr的相互作用，并分离了7和8的氢键配合物（H-TMG：HOAr）。成功分离1-6后，研究了1，2、4和5作为4-戊炔-1-醇分子内氢烷氧基化反应的前催化剂的用途。根据元素分析，FT-IR光谱以及〜1H和〜（13）C NMR研究，发现所有配合物的散装粉末均与晶体结构一致。

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