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A metal-organic complex of divalent zinc ions and its preparation method and application

A technology of metal-organic complexes, applied in zinc organic compounds, organic compounds/hydrides/coordination complex catalysts, organic chemistry, etc., can solve the problems of catalyst recycling difficulties, environmental pollution, etc., and achieve easy recycling and reduce The effect of cost and synthesis method is simple

Inactive Publication Date: 2020-05-29
SHANDONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the inventors have found that zinc chloride still has the following disadvantages as a catalyst: on the one hand, it is difficult to recycle the catalyst; on the other hand, the catalyst pollutes the environment as a metal salt

Method used

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  • A metal-organic complex of divalent zinc ions and its preparation method and application
  • A metal-organic complex of divalent zinc ions and its preparation method and application
  • A metal-organic complex of divalent zinc ions and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] The preparation of organic ligand L, the specific preparation steps are as follows:

[0062] (1) In a 50ml single-necked round bottom flask, add 4-cyanopyridine (2.08g, 20mmol) and sodium azide (1.56g, 24mmol) and then add anhydrous ammonium chloride (1.28g, 24mmol), add N , N-dimethylformamide (ie DMF) 20ml, heating and stirring at 120°C for 48h, followed by TLC. After the reaction is completed, cool it down, then pour it into a beaker filled with a large amount of deionized water, adjust the pH to pH 5-6 by adding dilute hydrochloric acid dropwise with a dropper, heat slowly with an electric heating mantle, and evaporate to dryness to obtain a light pink intermediate. After drying at room temperature and weighing, 4.59 g of a light pink intermediate was obtained, with a yield of 61%.

[0063] (2)N 2 Under protection, intermediate A (3.53g, 24mmol), 3-chloromethylpyridine (4.14g, 25.2mmol), anhydrous potassium carbonate (16.56g, 120mmol) were added to a 250ml single-...

Embodiment 2

[0066] The preparation of organic ligand L, the specific preparation steps are as follows:

[0067] (1) In a 50ml single-necked round bottom flask, add 4-cyanopyridine (2.08g, 20mmol) and sodium azide (1.3g, 20mmol) and then add anhydrous ammonium chloride (1.07g, 20mmol), add N , N-dimethylformamide (ie DMF) 20ml, heating and stirring at 110°C for 44h, followed by TLC. After the reaction is completed, cool it down, then pour it into a beaker filled with a large amount of deionized water, adjust the pH to pH 5-6 by adding dilute hydrochloric acid dropwise with a dropper, heat slowly with an electric heating mantle, and evaporate to dryness to obtain a light pink intermediate. Dry at room temperature and weigh to obtain 4.32 g of a light pink intermediate with a yield of 58%.

[0068] (2)N 2 Under protection, intermediate A (3.53g, 24mmol), 3-chloromethylpyridine (3.94g, 24mmol), anhydrous potassium carbonate (13.248g, 96mmol), potassium iodide (1.56g ,9.4mmol), then add 60....

Embodiment 3

[0070] The preparation of organic ligand L, the specific preparation steps are as follows:

[0071] (1) In a 50ml single-necked round bottom flask, add 4-cyanopyridine (2.08g, 20mmol) and sodium azide (1.95g, 30mmol) and then add anhydrous ammonium chloride (1.6g, 30mmol), add N , N-dimethylformamide (ie DMF) 20ml, heating and stirring at 130°C for 52h, followed by TLC. After the reaction is completed, cool it down, then pour it into a beaker filled with a large amount of deionized water, adjust the pH to pH 5-6 by adding dilute hydrochloric acid dropwise with a dropper, heat slowly with an electric heating mantle, and evaporate to dryness to obtain a light pink intermediate. After drying at room temperature and weighing, 4.7 g of a light pink intermediate was obtained, with a yield of 60%.

[0072] (2)N 2 Under protection, intermediate A (3.53g, 24mmol), 3-chloromethylpyridine (5.91g, 36mmol), anhydrous potassium carbonate (19.872g, 144mmol), potassium iodide (1.56g ,9.4mm...

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PUM

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Abstract

The invention relates to a metal organic complex of divalent zinc ions and a preparation method and application of the metal organic complex. An organic ligand L is prepared at first, and the structural formula is as shown in specification, the solution of the organic ligand L reacts with a zinc salt solution at room temperature to obtain a metal organic complex, and the metal organic complex hasa good catalytic effect in reaction of catalytic synthesis of diisopropylidene-D-mannitol as a catalyst.

Description

technical field [0001] The invention belongs to the technical field of functional complexes, and in particular relates to a kind of metal-organic complexes based on divalent zinc ions which can be loaded with dichloromethane or chloroform, and a preparation method and application thereof. Background technique [0002] The information disclosed in this background section is only intended to increase the understanding of the general background of the present invention, and is not necessarily taken as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to those skilled in the art. [0003] Metal-organic complexes (metal-organic complexes, MOCs) are research hotspots in recent years. Compared with traditional organic porous materials and inorganic porous materials, MOCs have a variety of adjustable structures and adjustable pores. The functionalized complexes showed great advantages in adsorption separation, fluorescence, biol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D401/14C07F3/06B01J31/22C07D317/20
CPCB01J31/1815B01J2531/26C07D317/20C07D401/14C07F3/06
Inventor 王建成刘建成贾万赫董育斌
Owner SHANDONG NORMAL UNIV
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