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Amino aryloxy rare earth metal amide and application thereof

A technology of aminoaryloxy rare earth and amides, which is applied to lithium organic compounds, compounds of group 4/14 elements of the periodic table, compounds containing elements of group 3/13 of the periodic table, etc., to achieve the effect of simple synthesis process

Inactive Publication Date: 2009-12-16
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] So far, in the application of rare earth metal complexes reported in the literature to catalyze the ring-opening polymerization of cyclic esters, there is no report on the use of aminoaryloxy rare earth metal amides as a single-component catalyst to catalyze the ring-opening polymerization of L-lactide

Method used

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  • Amino aryloxy rare earth metal amide and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Example 1: Preparation of [NO] 2 NdN(SiMe 3 ) 2 Li 2 (THF) 2 , [NO]=p-R 1 -C 6 H 4 NCH 2 (3-R 2 -5-R 3 -C 6 H 2 -2-O), R 1 is methyl, R 2 , R 3 Both are tert-butyl groups.

[0039] (1) 1.61 g of [NO]H 2 (4.95 mmol) was dissolved in tetrahydrofuran, added with Nd[N(SiMe 3 ) 2 ] 3 (μ-Cl)Li(THF) 3 (4.95 mmol) in tetrahydrofuran solution, the system was blue, and the reaction was stirred at 25°C overnight;

[0040] (2) Remove the solvent, add 30 ml of toluene for heating extraction, centrifuge, transfer the clear liquid, add 4.00 ml of hexane, concentrate the solution to 20 ml, overnight at room temperature, 2.22 g (2.00 mmol) of blue crystals are precipitated, and the yield is 41 %.

Embodiment 2

[0041] Example 2: Preparation of [NO] 2 YbN(SiMe 3 ) 2 Li 2 (THF) 2 , [NO]=p-R 1 -C 6 H 4 NCH 2 (3-R 2 -5-R 3 -C 6 H 2 -2-O), R 1 is methyl, R 2 , R 3 Both are tert-butyl groups.

[0042] (1) will contain 0.72 g [NO]H 2 (2.21 mmol) in tetrahydrofuran was added to a solution containing 2.21 mmol of Yb[N(SiMe 3 ) 2 ] 3 (μ-Cl)Li(THF) 3 In the tetrahydrofuran solution, the system was yellow, and the reaction was stirred at 25 °C overnight;

[0043] (2) The tetrahydrofuran solvent was removed, 20 ml of toluene was added for heating extraction, centrifugation, and the clear liquid was transferred, 3.00 ml of hexane was added, the solution was concentrated to 20 ml, and 1.04 g (0.91 mmol) of bright yellow crystals were precipitated at room temperature overnight. The yield was was 41%.

Embodiment 3

[0044] Example three, preparation of [NO] 2 SmN(SiMe 3 ) 2 Li 2 (THF) 2 , [NO]=p-R 1 -C 6 H 4 NCH 2 (3-R 2 -5-R 3 -C 6 H 2 -2-O), R 1 is methyl, R 2 , R 3 Both are tert-butyl groups.

[0045] (1) will contain 1.49 g [NO]H 2 (4.58 mmol) in tetrahydrofuran was added to a solution containing 4.58 mmol of Sm[N(SiMe 3 ) 2 ] 3 (μ-Cl)Li(THF) 3 In the tetrahydrofuran solution, the system was yellow, and the reaction was stirred at 25 °C overnight;

[0046] (2) The tetrahydrofuran solvent was removed, 40 ml of toluene was added for heating extraction, centrifugation, and the clear liquid was transferred, 5.00 ml of hexane was added, the solution was concentrated to 30 ml, and a large amount of yellow crystals, 2.38 g (2.14 mmol), were precipitated at room temperature. The yield was 46%.

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Abstract

The invention discloses an amino aryloxy rare earth metal amide and application thereof. The general formula of the amino aryloxy rare earth metal amide is [NO]2LnN(SiMe3)2Li2(THF)2, wherein Ln is a rare earth metal; and [NO]=p-R-C6H4NCH2(3-R-5-R-C6H2-2-O), R is selected from one of hydrogen or saturated alkyl groups of C1 to C4, and R and R are selected from one of methyl groups or tertiary butyl groups. The amino aryloxy rare earth metal amide can be used as a monocomponent catalyst to highly actively catalyze the ring-opening polymerization of L-lactide under mild conditions to obtain poly (L-lactide) with high molecular weight and proper molecular weight distribution.

Description

technical field [0001] The invention relates to a rare earth metal complex containing N, O double anion ligands, in particular to an aminoaryloxy rare earth metal amide and its catalytic application. Background technique [0002] Aliphatic polyester is a kind of biodegradable polymer material, 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, such as: polycaprolactone, because of its high solubility, low melting point, and compatibility with a variety of polymers, can be used as a polymer Plasticizers, etc.; polylactic acid, which is widely used in drug controlled release systems, orthopaedic fixation materials, and tissue engineering scaffold materials because of its characteristics. In view of some broad application prospects of aliphatic polyesters, its research has received extensive attention. [0003] Ring-opening polymerization is a...

Claims

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Application Information

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IPC IPC(8): C07F19/00C07F5/00C07F7/10C07F1/02C08G63/08C08G63/84C08G63/83
Inventor 姚英明卢敏沈琪
Owner SUZHOU UNIV
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