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Metal complex ligand, metal complex, preparation method and application thereof, high molecular polymer, preparation method and application thereof

A metal complex, complex technology, applied in the direction of organic compound/hydride/coordination complex catalyst, one-component synthetic polymer rayon, non-metallic conductor, etc.

Active Publication Date: 2014-08-20
ZANNAN SCITECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the shortcomings of existing olefin metathesis reaction catalysts and related olefin catalytic metathesis ring-opening polymerization reactions, the invention improves the mechanical properties of olefin polymerization products such as strength and modulus by developing and improving the performance of olefin metathesis reaction catalysts

Method used

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  • Metal complex ligand, metal complex, preparation method and application thereof, high molecular polymer, preparation method and application thereof
  • Metal complex ligand, metal complex, preparation method and application thereof, high molecular polymer, preparation method and application thereof
  • Metal complex ligand, metal complex, preparation method and application thereof, high molecular polymer, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0263] The synthesis of embodiment 1 ruthenium complex 4a

[0264] A 50mL two-neck flask was replaced with argon, and then added ligand 3a (10mmol), CuCl (30mmol, 3eq) and 30mL of dry DCM in sequence, and then replaced with argon three times, and then protected the closed system with an argon balloon. Ruthenium complex 1b (12 mmol) was added under the protection of argon, and reacted at room temperature for 0.5 hours. After the reaction was completed, silica gel was added to the filtrate to make sand, and the crude product was obtained by silica gel column chromatography, and then washed with methanol or pentane-DCM to obtain the green solid product 4a, the yield: 32%.

[0265] After detection, the ruthenium complex (4a) 1 HNMR (400MHz, CDCl 3 ): δ18.68 (s, Ru=CH), 7.23-6.65 (m, 10H, aromatic H), 6.36 (dd, J=2.8, 9.6Hz, 1H, aromatic H), 6.03 (d, J=12.8Hz , 1H, NCH 2 ), 4.14-3.90 (m, 4H, NCH 2 CH 2 N), 3.85(s, 3H, OCH 3 ), 3.47 (d, J=12.8Hz, 1H, NCH 2 ), 2.89-1.62 (m, 1...

Embodiment 2

[0266] The synthesis of embodiment 2 ruthenium complexes 4b:

[0267] A 50mL two-necked flask was replaced with argon, and then added ligand 3b (10mmol), CuCl (30mmol, 3eq) and 30mL of dry DCM in sequence, and then replaced with argon three times, and then protected the closed system with an argon balloon. Ruthenium complex 1a (12 mmol) was added under the protection of argon, and reacted at room temperature for 0.5 hours. After the reaction was completed, silica gel was added to the filtrate to make sand, and the crude product was obtained by silica gel column chromatography, and then washed with methanol or pentane-DCM to obtain the green solid product 4b, the yield: 35%.

[0268] After detection, the ruthenium complex (4b) 1 HNMR (400MHz, CDCl 3 ): δ19.28 (d, J = 8.4Hz, Ru = CH), 7.45 (d, J = 8.8Hz, 2H, aromatic H), 7.31-7.16 (m, 3H, aromatic H), 6.83 (d, J =8.8Hz, 2H, aromatic H), 5.13(t, J=12.4Hz, 1H, NH), 7.96(d, J=12.4Hz, 1H, NCH 2 ), 3.85 (d, J=12.4Hz, 1H, NCH 2 )...

Embodiment 3

[0269] The synthesis of embodiment 3 ruthenium complex 4c:

[0270]A 50mL two-necked flask was replaced with argon, and then added ligand 3c (10mmol), CuCl (30mmol, 3eq) and 30mL of dry DCM in sequence, and then replaced with argon three times, and then protected the closed system with an argon balloon. Ruthenium complex 1b (12 mmol) was added under the protection of argon, and reacted at room temperature for 0.5 hours. After the reaction was completed, silica gel sand was added to the filtrate after filtration, and the crude product was obtained by silica gel column chromatography, and then washed with methanol or pentane-DCM to obtain the green solid product 4c, the yield: 14%.

[0271] After detection, the ruthenium complex (4c) 1 HNMR (400MHz, CDCl 3 ): δ18.99 (s, Ru=CH), 7.483-7.444 (m, 1H, aromatic H), 7.192-6.862 (m, 7H, aromatic H), 6.715-6.662 (m, 1H, aromatic H), 5.293 (t, J=13.2Hz, 1H, NHCH 2 ), 4.19-3.58 (m, 8H, NHCH 2 , NCH 2 CH 2 N, NCH 3 ), 2.52-2.37 (m,...

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Abstract

The invention discloses a metal complex ligand, a metal complex, a preparation method and application thereof. Structural formulas of the metal (M) complex ligand Ia-Ic and the metal complex IIa-IIc thereof are shown in the description. The metal complex has the advantages of higher catalytic activity, diversity of structures and physical properties and the like, and provides diverse optimal selection to catalytic application of various raw materials. The invention also discloses various novel functional polymer materials generated by ring-opening metathesis polymerization (ROMP) of different types of small molecular cycloolefines and application thereof, and structures of the materials are shown below.

Description

technical field [0001] The present invention relates to a ligand, a complex and its preparation method and application, a polymer and its preparation method and application, in particular to a metal complex ligand, a metal complex and its preparation method and Application, a high molecular polymer and its preparation method and application. Background technique [0002] The research and development of olefin metathesis metathesis ruthenium catalysts and the use of new high-efficiency ruthenium complex catalysts to prepare various high-strength, high-hardness and other multi-functional polymer new materials through the method of olefin-catalyzed metathesis ring-opening polymerization (ROMP: Ring Opening Metathesis Polymerization) have attracted attention. received extensive attention. In this field, Grubbs, the founder of ruthenium complex catalysts, and other research groups have reported different types of ruthenium complex catalysts and the preparation of various rutheni...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C217/84C07C211/48C07C211/52C07C311/37C07C251/24C07C229/18C07C229/60C07C69/78C07C205/57C07C69/82C07C43/166C07D213/68C07F7/18C07C43/215C07C205/34C07C69/708C07C43/225C07C205/37C07F15/00B01J31/24B01J31/22C07D207/20C07D311/04C08G61/08C08G61/12C08L65/00D01F6/96A61K47/48A61K6/087C09K19/38H01B1/12A61K6/891A61K47/59
CPCB01J31/22B01J2231/543B01J2531/821C07D207/48C07D311/04C07D311/58C07F15/0046C08G61/08C08G61/12C08L65/00D01F6/96
Inventor 詹正云
Owner ZANNAN SCITECH
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