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A kind of fullerene derivative micron flower and preparation method thereof

A technology of fullerene derivatives and micron flowers, applied in the direction of organic chemistry, can solve the problems of affecting the effect, the product scale of micron flower shape cannot be adapted to the application, and the content of compounds is low.

Active Publication Date: 2018-10-12
HUANGSHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] However, it has been found in practical applications that in the crystalline product of N-methyl-2-[4-dimethylamino]phenyl-3,4-fullerenylpyrrolidine microflowers prepared by the method, the The content of the compound is low, which affects the effect of the actual application process; in addition, the scale of the micron flower form product obtained by this method is also unable to adapt to more applications

Method used

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  • A kind of fullerene derivative micron flower and preparation method thereof
  • A kind of fullerene derivative micron flower and preparation method thereof
  • A kind of fullerene derivative micron flower and preparation method thereof

Examples

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Embodiment 1

[0028] The preparation of embodiment 1N-methyl-2-[4-dimethylamino] phenyl-3,4-fullerenyl pyrrolidine

[0029] The preparation method of N-methyl-2-[4-dimethylamino]phenyl-3,4-fullerenylpyrrolidine described in this example is prepared according to known methods in the prior art, specifically: Under the protection of argon, the fullerene C was first mixed with a molar ratio of 1:7 60 Dissolve in freshly distilled toluene and stir for 1-2h to give fullerene C 60 toluene solution, and then to the fullerene C 60 Add 4-dimethylaminobenzaldehyde and sarcosine to the toluene solution, and place it under reflux at 120°C for 2-3 hours to obtain a reaction solution, wherein the fullerene C in the reaction solution 60 The molar ratio of , 4-dimethylaminobenzaldehyde and sarcosine is 1:5:3, and then, argon gas is introduced into the reaction solution, and after cooling to room temperature, it is filtered, concentrated and columnar. Chromatographic separation to obtain the reaction conc...

Embodiment 2

[0031] The preparation method of N-methyl-2-[4-dimethylamino]phenyl-3,4-fullerenylpyrrolidine micron flower described in this example comprises the following steps:

[0032] (1) 0.5 g of N-methyl-2-[4-dimethylamino]phenyl-3,4-fullerenylpyrrolidine prepared in Example 1 was mixed with 1L of carbon tetrachloride solvent, Prepare a solution of N-methyl-2-[4-dimethylamino]phenyl-3,4-fullerenylpyrrolidine carbon tetrachloride with a concentration of 0.5g / L for subsequent use;

[0033](2) Get cetyltrimethylammonium bromide and isopropanol solvent and mix, and the obtained concentration is the cetyltrimethylammonium bromide isopropanol solution of 10mmol / L, for subsequent use;

[0034] (3) Get the N-methyl-2-[4-dimethylamino]phenyl-3,4-fullerenylpyrrolidine carbon tetrachloride prepared in step (1) according to the volume ratio of 1:1 solution, mixed with the cetyltrimethylammonium bromide isopropanol solution prepared in step (2) and stirred, the temperature of the reaction system ...

Embodiment 3

[0037] The preparation method of N-methyl-2-[4-dimethylamino]phenyl-3,4-fullerenylpyrrolidine micron flower described in this example comprises the following steps:

[0038] (1) Take N-methyl-2-[4-dimethylamino]phenyl-3,4-fullerenyl pyrrolidine 3g prepared in Example 1 and mix with 1L carbon tetrachloride solvent to prepare The N-methyl-2-[4-dimethylamino]phenyl-3,4-fullerenylpyrrolidine carbon tetrachloride solution with a concentration of 3.0 g / L was prepared for subsequent use;

[0039] (2) Get cetyltrimethylammonium bromide and isopropanol solvent and mix, and the obtained concentration is the cetyltrimethylammonium bromide isopropanol solution of 2mmol / L, for subsequent use;

[0040] (3) Get the N-methyl-2-[4-dimethylamino]phenyl-3,4-fullerenylpyrrolidine carbon tetrachloride prepared in step (1) according to the volume ratio of 1:10 solution, mixed with the cetyltrimethylammonium bromide isopropanol solution prepared in step (2) and stirred, the temperature of the react...

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Abstract

The invention belongs to the technical field of compound preparation, particularly relates to a fullerene derivative microflower and further discloses a preparation method of the fullerene derivative microflower. The preparation method is based on the known surfactant assisted self-assembly method in the prior art and is further developed. The stirring condition of a N-methyl-2-(4-dimethyl amidogen) phenyl-3,4-fullerene pyrrolidine carbon tetrachloride solution and a hexadecyl trimethyl ammonium bromide isopropanol solution is optimized, and the obtained N-methyl-2-(4-dimethyl amidogen) phenyl-3,4-fullerene pyrrolidine microflower is of a spherical flower-shaped structure, the spherical flower is composed of curved surface microsheets standing in a mutually-crossed mode, and the microsheets are of a single crystalline structure and are 1-2 micrometers long, 1-2 micrometers high and 10-20 manometers thick.

Description

technical field [0001] The invention belongs to the technical field of compound preparation, specifically relates to a fullerene derivative micron flower, and further discloses a preparation method thereof. Background technique [0002] In 1985, when scientists such as R.F.Crul, R.E.Smallay and H.W.Kroto of the United Kingdom used high-energy laser pulses to graphite, they accidentally discovered a series of carbon ion clusters represented by C60, which were later called fullerenes or football enes. Fullerene thus stands out as the third allotrope of carbon. Later, inspired by the vaulted dome designed by architectural designer Buckminster Fuller, Kroto and others finally determined that C60 has a closed spherical cage structure similar to the vaulted dome, which is consistent with the "stable" structure of C60. matching in nature. [0003] In the research on fullerenes, the application of fullerenes has always been one of the main topics that scientists are most concerned...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D209/96
CPCC07D209/96
Inventor 黄飞魏先文
Owner HUANGSHAN UNIV
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