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Preparation method of fullerene-polyoxometalate hybrid molecule

A polyoxometalate, fullerene technology, applied in the direction of organic chemistry, can solve the problem of difficult chemical modification, and achieve the effect of strong designability, novel structure and strong functionality

Active Publication Date: 2018-06-29
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

First of all, fullerenes and polyoxometalates are both nanoscale rigid frameworks, and it is very difficult to chemically modify them

Method used

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  • Preparation method of fullerene-polyoxometalate hybrid molecule
  • Preparation method of fullerene-polyoxometalate hybrid molecule
  • Preparation method of fullerene-polyoxometalate hybrid molecule

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) Take 9.87 mmol p-hydroxybenzaldehyde, 14.88 mmol anhydrous K 2 CO 3 In a 100 ml two-necked bottle, vacuumize and vent argon, repeat three times, inject N,N-dimethylformamide solution (40 ml) containing 12.84 mmoles of bromoacetate tert-butyl therein, 70 o C overnight. Filter to remove potassium carbonate, concentrate, transfer the concentrated solution to a separatory funnel, extract three times with ethyl acetate, combine the organic phases, dry over anhydrous magnesium sulfate, filter with suction, take the filtrate, and remove the organic solvent under reduced pressure. Dissolve the crude product in a small amount of n-hexane / ethyl acetate mixed solvent (the volume ratio of ethyl acetate is 30%), and use this as eluent for silica gel column chromatography to obtain tert-butyl acetate substituted Benzaldehyde. Pale yellow solid with a yield of 70.39%.

[0042] (2) Add 2.54 mmol C 60 and 8.50 mmoles of sarcosine, vacuumize, and flow argon, repeat three times, ...

Embodiment 2

[0056] On the basis of Example 1, the p-hydroxybenzaldehyde in step (1) was replaced by 2,4-dihydroxybenzaldehyde, the amount of tert-butyl bromoacetate was adjusted to 25.68 mmol, anhydrous K 2 CO 3 The amount of addition is adjusted to 20 mmoles; Dawson-NH in step 4 2 The addition amount of is adjusted to 0.80 mmol, and other conditions are unchanged.

Embodiment 3

[0058] On the basis of Example 2, p-hydroxybenzaldehyde in step (1) was replaced by 2,5-dihydroxybenzaldehyde, and other conditions remained unchanged.

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Abstract

The invention discloses a preparation method of fullerenes-polyoxometalates hybrid molecules. According to the technical scheme, the preparation method comprises the following steps: firstly, taking bromoalkyl acid tert-butyl ester to replace benzaldehyde, sarkosine and fullerenes as the raw materials, taking chloro benzene as a solvent, and carrying out [3+2] cycloaddition reaction to prepare fullerene derivatives containing tert-butyl ester; and further hydrolyzing the fullerene derivatives containing the tert-butyl ester to obtain fullerene derivatives containing carboxyl, and then carrying out amidation reaction on the fullerene derivatives containing the carboxyl and polyoxometalates containing amino so as to attach the fullerene derivatives containing the carboxyl to the polyoxometalates containing the amino together in a covalent manner. The preparation method of the fullerenes-polyoxometalates hybrid molecules is simple to operate, and types and numbers of the fullerenes and the polyoxometalates in target molecules are adjustable.

Description

technical field [0001] The invention belongs to the field of new materials and relates to a preparation method of fullerene-polyoxometalate hybrid molecules. Background technique [0002] Polyoxometalates are metal oxygen cluster compounds formed by bridging transition metal elements (mainly molybdenum, tungsten, vanadium) and oxygen atoms. The basic unit of metal oxygen clusters is mainly MO 4 Tetrahedra and MO 6 Octahedron, different polyhedrons are further connected by sharing edges, corners or planes to form complex and diverse polyacid structures. Polyoxometalates have many peculiar properties, such as oxidation, strong acidity, large size, high negative charge, nucleophilic properties, etc., and are widely used in catalysis, medicine, electrochemistry, photochromism and magnetism The field shows great application potential, so it has aroused great interest and attention. However, due to the high lattice energy and low pH stability of polyoxometalates, it is very di...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D209/58
CPCC07D209/58
Inventor 李洪光周升菊冯永强刘宝勇
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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