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Method for preparing [60] fullerene dihydropyridine-3-ketone derivative through catalysis of p-methoxybenzoic acid and copper acetate and product

A technology of fullerene dihydropyridine and methoxybenzoic acid is applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc. Novel, simple raw materials, mild reaction conditions

Active Publication Date: 2022-05-27
HUBEI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] These methods for synthesizing fullerene nitrogen-oxygen heterocyclic structures have some limitations, such as complex reactions, difficult access to raw materials, etc., so further explore the synthesis method of fullerene nitrogen-oxygen heterocyclic structures with simple reactions and cheap and easy-to-obtain raw materials is very necessary

Method used

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  • Method for preparing [60] fullerene dihydropyridine-3-ketone derivative through catalysis of p-methoxybenzoic acid and copper acetate and product
  • Method for preparing [60] fullerene dihydropyridine-3-ketone derivative through catalysis of p-methoxybenzoic acid and copper acetate and product
  • Method for preparing [60] fullerene dihydropyridine-3-ketone derivative through catalysis of p-methoxybenzoic acid and copper acetate and product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] [60] Preparation of fullerene dihydropyridin-3-one derivative 1:

[0056]

[0057] The specific preparation steps are:

[0058] [60]fullerene (36.0 mg, 0.05 mmol), 4-methoxyphenethylamine (37 μL, 0.25 mmol), p-methoxybenzoic acid (38.0 mg, 0.25 mmol), copper acetate monohydrate (39.9 mg, 0.20 mmol) were added to a round bottom flask. 6 mL of o-dichlorobenzene was added, and the mixture was completely dissolved by ultrasonication. Then, the mixture was immediately placed in an oil bath with a preset temperature of 100 ° C, heated and stirred for 300 minutes, and the reaction process was detected by thin-layer chromatography (TLC). Tracking, the product no longer increases at the point plate, and the reaction is stopped when the by-product at the origin gradually increases. After the reaction, the reaction mixture was coarsely filtered through a short silica gel column to remove metal salts and insoluble impurities. The solvent was spun out under reduced pressure in...

Embodiment 2

[0061] [60] Preparation of fullerene dihydropyridin-3-one derivative 2:

[0062]

[0063] The specific preparation steps are:

[0064] [60]fullerene (36.0 mg, 0.05 mmol), 4-methylphenethylamine (36 μL, 0.25 mmol), p-methoxybenzoic acid (38.0 mg, 0.25 mmol), copper acetate monohydrate (39.9 mg, 0.20 mmol) were added to a round bottom flask. 6 mL of o-dichlorobenzene was added, and the mixture was completely dissolved by ultrasonication. Then, the mixture was immediately placed in an oil bath with a preset temperature of 100 ° C and heated and stirred for 280 minutes. The reaction process was spotted by thin-layer chromatography (TLC). Tracking, the product no longer increases at the point plate, and the reaction is stopped when the by-product at the origin gradually increases. After the reaction, the reaction mixture was coarsely filtered through a short silica gel column to remove metal salts and insoluble impurities. The solvent was spun out under reduced pressure in a ...

Embodiment 3

[0067] [60] Preparation of fullerene dihydropyridin-3-one derivative 3:

[0068]

[0069] The specific preparation steps are:

[0070] [60]fullerene (36.0 mg, 0.05 mmol), 4-chlorophenethylamine (35 μL, 0.25 mmol), p-methoxybenzoic acid (38.0 mg, 0.25 mmol), copper acetate monohydrate (39.9 mg, 0.20 mmol) were added to a round bottom flask. 6 mL of o-dichlorobenzene was added, and the mixture was completely dissolved by ultrasonication. Then, the mixture was immediately placed in an oil bath with a preset temperature of 100 ° C and heated and stirred for 180 minutes. The reaction process was spotted by thin-layer chromatography (TLC). Tracking, the product no longer increases at the point plate, and the reaction is stopped when the by-product at the origin gradually increases. After the reaction, the reaction mixture was coarsely filtered through a short silica gel column to remove metal salts and insoluble impurities. The solvent was spun out under reduced pressure in a ...

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Abstract

The invention belongs to the technical field of organic synthesis, and particularly relates to a method for preparing a [60] fullerene dihydropyridine-3-ketone derivative based on catalysis of p-methoxybenzoic acid and copper acetate and a product. According to the method, [60] fullerene and an arylethylamine derivative are taken as raw materials, p-methoxybenzoic acid and copper acetate are taken as catalysts, o-dichlorobenzene is taken as a solvent, and the [60] fullerene dihydropyridine-3-ketone derivative is obtained through oil bath heating reaction in air. The novel fullerene dihydropyridine-3-ketone derivative is prepared by reacting [60] fullerene with the arylethylamine derivative, so that the yield of a target product is increased, and the selectivity of the product is improved.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a method and a product for preparing [60]fullerene dihydropyridin-3-one derivatives based on p-methoxybenzoic acid and copper acetate catalyzed. Background technique [0002] The special structure and unique physical and chemical properties of fullerenes have always attracted the attention of scientific researchers. However, due to the all-carbon cage structure of fullerene itself, it has basically no polarity. This feature makes fullerene very poor in solubility in water and polar organic solvents, which limits the application of fullerene in many fields. development and application. It is an important method to study fullerene chemistry by attaching various functional groups to the fullerene carbon skeleton through chemical modification, which can change the surface structure of fullerene and Various physical and chemical properties enable it to be better applied to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D221/18C07D409/14B01J31/22
CPCC07D221/18C07D409/14B01J31/2213B01J2531/16Y02P20/584
Inventor 吴非仑柴明顶王兴宇李法宝
Owner HUBEI UNIV
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