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Amino aryloxy rare earth metal complex, preparation thereof and application thereof

An amino aryloxy rare earth, metal complex technology, applied in organic compounds/hydrides/coordination complex catalysts, compounds containing periodic table Group 3/13 elements, chemical instruments and methods, etc. The problems of synthesis and low catalytic performance of aryloxy rare earth metal complexes can achieve the effect of high yield, convenient method and high activity.

Inactive Publication Date: 2011-09-21
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] There are relatively few studies on the synthesis and catalytic performance of aminoaryloxy rare earth metal complexes reported in the literature

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1: {[NO]LaN(TMS) 2 } 2 (R 1 = R 2 = Bu t )Synthesis

[0035] Ligand [NO]H 2 (0.68 g, 2.00 mmol) of toluene solution was added to La(N(TMS) 2 ] 3 (μ-Cl)Li(THF) 3 In the toluene solution (1.75 g, 2.00 mmol), the colorless clear solution gradually changed to yellow turbid solution, and the solution was stirred at 80°C overnight. Centrifuge while hot, remove the precipitate, transfer the clear solution, and concentrate. After a few days at room temperature, 1.39 grams of colorless crystals are precipitated, and the yield is 95%. {[NO]LaN(TMS) 2 } 2 Infrared spectrum (KBr, cm -1 ): 3635(s), 2945(s), 2336(m), 1604(s), 1535(s), 1458(m), 1358(m), 1290(w), 1200(s), 1150(w ), 1086(s), 1083(m), 860(w), 836(s), 745(s), 553(m). NMR: 1 H NMR (400 MHz, d 8 -THF): 7.05-7.20(m, Ar-CH 3 ); 7.02-7.04(m, 2H, Ar); 6.98-7.02(m, 2H, Ar); 6.66-6.71(m, 4H, Ar); 6.42-6.45(m, 2H, Ar); 6.01-6.06( m, 2H, Ar); 4.18(s, 4H, CH2); 4.10(s, 6H, OCH3); 2.30(s, Ar-CH3); 1.44(s, 18H, tBu-Ar); 1....

Embodiment 2

[0036] Embodiment 2: {[NO]NdN(TMS) 2 } 2 (R 1 = R 2 = Bu t )Synthesis

[0037] Ligand [NO]H 2 (0.68 g, 2.00 mmol) of toluene solution was added to Nd(N(SiMe 3 ) 2 ] 3 (μ-Cl)Li(THF) 3 In the toluene solution (1.76 g, 2.00 mmol), the clear blue-purple solution gradually turned into a blue-green turbid solution, and the solution was stirred at 80°C overnight. Centrifuge while hot, remove the precipitate, transfer the clear solution, and concentrate. After a few days at room temperature, 1.37 g of blue crystals are precipitated, and the yield is 93%. {[NO]NdN(TMS) 2 } 2 Infrared spectrum (KBr, cm -1 ): 3650(s), 2958(s), 2466(s), 1640(s), 1508(s), 1458(s), 1419(m), 1358(m), 1300(w), 1245(s) ), 1172(w), 1122(s), 1022(m), 883(w), 836(s), 748(s), 532(m). Elemental analysis: C, 57.21%; H, 7.69%; Nd, 19.45%; N, 3.76%. The above data proves that the target compound was successfully prepared.

Embodiment 3

[0038] Example 3: {[NO]SmN(TMS) 2 } 2 (R 1 = Bu t , R 2 = Me) synthesis

[0039] Ligand [NO]H 2 (0.65 g, 2.00 mmol) of toluene solution was added to Sm(N(SiMe 3 ) 2 ] 3 (μ-Cl)Li(THF) 3 In the toluene solution (1.77 g, 2.00 mmol), the color of the solution gradually changed from yellow to red turbid solution, stirred at 70°C overnight. Centrifuge while hot, remove the precipitate, transfer the clear liquid, and concentrate. After a few days at room temperature, 1.34 g of red crystals are precipitated, and the yield is 90%. {[NO]SmN(TMS) 2 } 2 Infrared spectrum (KBr, cm -1 ): 3700(s), 2954(s), 2450(s), 1600(s), 1477(s), 1358(m), 1230(m), 1246(s), 1169(w), 1122(s) ), 984(m), 933(s), 836(s), 744(s), 602(s), 521(m). Elemental analysis: C, 56.66%; H, 7.54%; Sm, 20.21%; N, 3.69%. The above data proves that the target compound was successfully prepared.

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PUM

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Abstract

The invention discloses an amino aryloxy rare earth metal complex. The technical scheme adopted by the invention is as follows: the amino aryloxy rare earth metal complex is an o-methoxyphnol amino aryloxy rare earth metal amide whose general formula is {[NO]LnN(TMS)2}2, wherein Ln is one respectively selected from the group of lanthanum, neodymium, samarium, ytterbium and yttrium; [NO] is o-OCH<3>-C6H4NCH2(3-R1-5-R2-C6H2-2-O), wherein R1 and R2 is one selected from the group of methyl and t butyl; The amino aryloxy rare earth metal complex has the advantages of convenient synthesis and high productivity. And the amino aryloxy rare earth metal complex can catalyze the polymerization of lactide as a monocomponent catalyst under mild condition to obtain a high molecular weight polymer. The rare earth metal complex has the advantages of convenient synthesis and high catalytic activity.

Description

Technical field [0001] The invention belongs to the field of amino aryloxy complexes, and specifically relates to an o-methoxyamino aryloxy rare earth metal amide and its catalytic application. Background technique [0002] Aliphatic polyester is a class of biodegradable polymer materials, which can be degraded under physiological conditions, and the degradation products are non-toxic. Therefore, it has been used clinically as a compatible material for biological tissues (see: Hayashi, T. Prog. Polym. Sci., 1994, 19, 663). Polylactic acid has high solubility, low melting point, and is compatible with a variety of polymers, and can be used as a plasticizer for polymers. Its characteristics have been widely used in drug controlled release systems (see: Zhang, XC; McAuley, KB; Gossen, MFAJ Control. Release 1995, 34, 175), orthopedic fixation materials (see: Bergsm, JE; RoZem, FR; Bos, RM et al Joral. Maxillofac. Surg. 1993, 51, 666), and tissue engineering Scaffold materials (see:...

Claims

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Application Information

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IPC IPC(8): C07F5/00B01J31/22C08G63/08C08G63/84
Inventor 姚英明张洁邱金水王超沈琪
Owner SUZHOU UNIV
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