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Rare earth-lithium heterobimetallic complex, synthesizing method and use thereof

A technology of metal amides and rare earths, which is applied in the field of rare earth-lithium double metal complexes, can solve the problems of few research reports on the catalytic performance of bridged double rare earth metal complexes and no activity, and achieve convenient synthesis and high yield Effect

Inactive Publication Date: 2009-08-12
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0020] However, so far, there are few reports on the synthesis and catalytic performance of bridged double rare earth metal complexes (Yuen, H.F.; Marks, T.J.Organometallics.2008, 27, 157)
In order to investigate the influence of double metals on the catalytic performance, we designed an imidazolidinyl bridged bis-aryloxy ligand and synthesized a double rare earth metal complex containing hexamethylphosphonic triamide (HMPA) coordination. But they show no activity for ring-opening polymerization of cyclic ester monomers (Xu, X.P.; Yao, Y.M.; Zhang, Y.; Shen, Q.Inorg.Chem.2007, 46, 3743)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Embodiment one: (THF)Li(μ-Cl)[(SiMe 3 ) 2 N] 2 Ln[OArNNArO]Ln[N(SiMe 3 ) 2 ] 2 Synthesis of (μ-Cl)Li(THF); the substituents at the 3 and 5 positions on the aromatic ring are tert-butyl and methyl respectively, Ln=Yb;

[0044] [OArNNArO]H 2 (1.00 g, 2.28 mmol) in tetrahydrofuran was added to Yb[N(SiMe 3 ) 2 ] 3 (μ-Cl)Li(THF) 3 (4.56 mmol) of tetrahydrofuran solution, the system changed from a brownish yellow solution to a yellow turbid solution first and then to a bright yellow transparent solution. Stir and react at 50°C for two nights, remove the tetrahydrofuran solvent, add 20 ml of toluene for heating and extraction, and centrifuge A little precipitate was removed, the supernatant was transferred, concentrated, and left overnight at room temperature, and 2.49 g (1.50 mmol, 66%) of bright yellow crystals were precipitated.

Embodiment 2

[0045] Embodiment two: (THF)Li(μ-Cl)[(SiMe 3 ) 2 N] 2 Ln[OArNNArO]Ln[N(SiMe 3 ) 2 ] 2 Synthesis of (μ-Cl)Li(THF); the 3 and 5 substituents on the aromatic ring are all tert-butyl, Ln=Yb;

[0046] [OArNNArO]H 2 (0.86 g, 1.65 mmol) in tetrahydrofuran was added to Yb[N(SiMe 3 ) 2 ] 3 (μ-Cl)Li(THF) 3 (3.13 millimoles) in THF solution, the reaction system changed from brownish-yellow solution to yellow turbid solution and then turned into bright yellow transparent solution, stirred and reacted at 50°C for two nights, removed THF solvent, added 25 milliliters of toluene for heating and extraction, A little precipitate was removed by centrifugation, the clear liquid was transferred, the toluene solvent was concentrated, and left at room temperature for two days, 2.01 g (1.16 mmol, 70%) of yellow crystals were precipitated.

Embodiment 3

[0047] Embodiment three: (THF)Li(μ-Cl)[(SiMe 3 ) 2 N] 2 Ln[OArNNArO]Ln[N(SiMe 3 ) 2 ] 2 Synthesis of (μ-Cl)Li(THF); the 3 and 5 substituents on the aromatic ring are all tert-butyl, Ln=Eu;

[0048] [OArNNArO]H 2 (1.22 g, 2.34 mmol) in tetrahydrofuran was added to Eu[N(SiMe 3 ) 2 ] 3 (μ-Cl)Li(THF) 3 (4.91 mmol) of tetrahydrofuran solution, the brick red reaction solution first became turbid and then slowly turned into a dark red transparent solution, stirred and reacted at 50°C for two nights, the tetrahydrofuran solvent was removed, 20 ml of toluene was added for heating and extraction, and centrifuged to remove After a little precipitation, the supernatant was transferred, the toluene solvent was concentrated, and left at room temperature for two days, 2.85 g (1.68 mmol, 72%) of dark red crystals were precipitated.

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Abstract

The invention discloses a piperazidine alkyl bridged bi-aryloxy rare earth-lithium bi-metal amide with a molecular formula of (THF)Li(mu-Cl)[(SiMe3)2N]2Ln[OArNNArO]Ln[N(SiMe3)2]2(mu-Cl)Li(THF) and a synthesizing method thereof, wherein the Ln is heavy rare earth metal which is selected from any one of the following substances: europium (Eu), erbium (Er) or ytterbium (Yb); and in [OArNNArO]=C4H8N2[1,4-(2-O-5-R-3-R-C6 H2CH2-)2], R and R are respectively selected from methyl or tert-butyl group. Piperazidine alkyl bridged bi-aryloxy rare earth-lithium catalysts provided by the invention can be used as single-component catalysts in a mild condition to catalyze the ring opening polymerization of L-lactide with high activity so as to obtain polylactide with high molecular weight and appropriate molecular weight distribution.

Description

technical field [0001] The invention relates to a rare earth-lithium double metal complex, in particular to a rare earth-lithium double metal complex containing two rare earth metals and a piperazinyl bridged bisaryloxy group. Background technique [0002] Since there may be a synergistic effect between the two metal centers in the bimetallic complexes, which may show unique catalytic performance, the synthesis of bimetallic complexes and their catalytic properties have aroused widespread interest. The bimetallic complexes reported in the literature can be divided into ligand-stabilized bimetallic complexes such as bridged amidino groups, bridged imino groups, Schiff bases, and bridged bisindenyl or cyclocene groups. [0003] Reports on the bridged amidino type: [0004] (1) In 1999, Sita et al first reported the reaction of inserting metal-carbon bonds through diimine, and synthesized bridged amidinotitanium bimetallic complexes (see: Rheingold, A.L.; Fettinger, J.C.; Sita...

Claims

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Application Information

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IPC IPC(8): C07F19/00C07F5/00C07F1/02C07D295/096C08G63/08C08G63/84C08G63/83
Inventor 姚英明张中剑孙松聂昆沈琪
Owner SUZHOU UNIV
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