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Preparation method and application of a class of porous organic polymers containing pyridine groups

A pyridine group, polymer technology, applied in the field of porous polymers and their preparation, porous organic polymers, can solve the problems of difficult recycling of catalysts, low catalyst activity, etc., achieve high catalytic activity and recyclability, preparation method Simple, high-yield effects

Active Publication Date: 2022-05-20
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there are still many difficulties to be overcome in the heterogeneous catalytic nitrogen formylation reaction: first, the activity of the catalyst is low; second, the recycling of the catalyst is difficult to solve

Method used

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  • Preparation method and application of a class of porous organic polymers containing pyridine groups
  • Preparation method and application of a class of porous organic polymers containing pyridine groups
  • Preparation method and application of a class of porous organic polymers containing pyridine groups

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Tris (4-vinylphenyl) phosphine used in the following examples is prepared by the following method, specifically:

[0031] Tris(4-vinylphenyl)phosphine preparation of

[0032] Magnesium (160mg, 1.2mmol) was cut into small pieces and placed in a three-necked flask that had been dried and connected to a constant pressure dropping funnel, and one piece of iodine was added, and the reaction system was sealed and replaced with a nitrogen system to ensure that there was no water in the system. oxygen. Add 4-bromostyrene (0.7mL, 1mmol) into the constant pressure dropping funnel, and add 20mL of anhydrous tetrahydrofuran. Slowly drop the mixed liquid in the constant pressure dropping funnel into the flask, heat and stir for 1 hour. The reaction system was transferred to an ice-water bath, phosphorus trichloride (0.15 mL, 0.3 mmol) was slowly added thereto with a syringe, and stirred overnight. After stirring overnight, add saturated ammonium chloride aqueous solution and ex...

Embodiment 2

[0034] Synthesis of Polymer I

[0035] Under a nitrogen atmosphere, anhydrous tetrahydrofuran (10.0 mL) was added to a 50 mL stopcock bottle, and the copolymerization unit (570.0mg, 1.68mol) and (35.3mg, 0.34mmol), and finally 5.0mg of initiator AIBN was added. After stirring at room temperature for 10 min, react at 100°C for 24 h, the product was separated by centrifugation, washed with tetrahydrofuran (3×6 mL) and rotary evaporated to give a light yellow solid (590.0 mg).

Embodiment 3

[0037] Synthesis of Porous Organic Polymer I Supported Ruthenium Catalyst Rh / I with Pyridine Groups as follows

[0038] Into a 100mL Schlenk tube, add (500.0 mg), RuCl 3 (71.8mg) and anhydrous tetrahydrofuran (8mL). After stirring at room temperature for 24 h, the reaction product was washed with anhydrous toluene and then centrifuged, and thus centrifuged three times. Finally, the toluene was removed by rotary evaporation under reduced pressure, and the oil pump was used for 3 h to obtain the catalyst Rh / I (570 mg).

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Abstract

The invention discloses a preparation method and application of a class of porous organic polymers containing pyridine groups. The polymer I has the following general formula: the above polymer is obtained by copolymerizing with and . The porous organic polymer containing pyridine group provided by the present invention and transition metal salt RuCl 3 The catalyst formed by complexation can be used to catalyze the nitrogen formylation reaction of amine, and has the advantages of high catalytic rate, good yield and recyclability.

Description

technical field [0001] The invention relates to a class of porous organic polymers containing pyridine groups, a preparation method and application thereof. Specifically, it relates to a class of porous polymers containing pyridine and triphenylphosphine ligands and a preparation method thereof. The polymer-loaded ruthenium catalyst can efficiently catalyze the nitrogen formylation reaction of amines, and belongs to the technical field of organic chemistry. [0002] technical background [0003] The nitrogen formylation reaction refers to the process in which an amine reacts with an acylating reagent to form a formamide. Formamide compounds can be used not only as solvents and reagents, but also as catalysts. CO 2 / H 2 As an acylating agent, the transition metal-catalyzed acylation of amines provides a class of green synthetic methods for the synthesis of carboxamides. Compared with the nitrogen formylation reaction of the homogeneous catalyst system, the nitrogen formyla...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G61/12B01J31/06B01J35/10B01J31/30C07B43/06C07D295/182C07C231/10C07C233/13C07C233/03C07C233/18
CPCC08G61/122C08G61/12B01J31/06B01J31/30C07B43/06C07D295/182C07C231/10C08G2261/122C08G2261/344C08G2261/3221B01J35/60C07C233/13C07C233/03C07C233/18Y02P20/584
Inventor 贾肖飞宗玲博张凯吕锦鹤张金荣宋嘉欣
Owner QINGDAO UNIV OF SCI & TECH