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Molybdenum-containing polyoxometalate and adamantane hybrid compound and preparation method thereof

A technology of polyoxometalate and adamantane is applied in the field of preparation of hybrid compounds to achieve the effects of easy control of the reaction process, simple purification and simple and easy preparation method.

Inactive Publication Date: 2012-01-04
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of hybrid compounds by covalently linking adamantane derivatives with polyoxometallic acids has not been reported yet.

Method used

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  • Molybdenum-containing polyoxometalate and adamantane hybrid compound and preparation method thereof
  • Molybdenum-containing polyoxometalate and adamantane hybrid compound and preparation method thereof
  • Molybdenum-containing polyoxometalate and adamantane hybrid compound and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0025] 1)[(n-Bu) 4 N] 4 Mo 8 o 26 Synthesis

[0026] 12.353g (NH 4 ) 6 (Mo 7 o 24 )·4H 2 O, 11.268g Bu 4 NBr was dissolved in 60ml deionized water respectively to obtain a colorless transparent solution. Under electromagnetic stirring, the dissolved Bu 4 NBr solution was added dropwise to (NH 4 )6 (Mo 7 o 24 )·4H 2 In the O solution, a white precipitate was formed. After the dropwise addition, continue to stir for 2 minutes. After suction filtration, wash with deionized water, acetone, and anhydrous ether to obtain a white solid. Dissolve it with 120ml of acetonitrile solvent at room temperature and freeze to obtain a colorless small piece. crystals, filtered and dried to obtain [(n-Bu) 4 N] 4 Mo 8 o 26 White solid 18.301g, yield 85%;

[0027] 2) Synthesis of N-trimethylolmethyl-adamantane carboxamide

[0028] Under argon protection, 2.32g of 1-adamantanecarboxylic acid, 4.77g of 2-ethoxyl-1-ethoxycarbonyl-1,2-dihydroquinoline (EEDQ), 2.49g of trishydroxymet...

Embodiment 2

[0034] 1)[(n-Bu) 4 N] 4 Mo 8 o 26 Synthesis

[0035] 12.353g (NH 4 ) 6 (Mo 7 o 24 )·4H 2 O, 11.268g of Bu4NBr were dissolved in 60ml of deionized water to obtain a colorless transparent solution. Under electromagnetic stirring, the dissolved Bu 4 NBr solution was added dropwise to (NH 4 ) 6 (Mo 7 o 24 )·4H 2 In the O solution, a white precipitate was formed, and the stirring was continued for 2 min after the dropwise addition. Suction filtration, washing with deionized water, acetone, and anhydrous ether respectively to obtain a white solid, which was dissolved with as little acetonitrile (120 ml) as possible at room temperature, and frozen to obtain small colorless crystals. Suction filtration, dry, obtain [(n-Bu) 4 N] 4 Mo 8 o 26 White solid 18.301g, yield 85%;

[0036] 2) Synthesis of N-trimethylolmethyl-adamantaneacetamide

[0037] Under argon protection, 1g adamantaneacetic acid, 1.91g 2-ethoxyl-1-ethoxycarbonyl-1,2-dihydroquinoline (EEDQ), 1g trishyd...

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Abstract

The invention discloses a molybdenum-containing polyoxometalate and adamantane hybrid compound, which is prepared by connecting molybdenum-containing polyoxometalate and adamantane through a covalent bond. The preparation method comprises the following synthesis steps of: 1) performing amidation reaction on adamantane carboxylic acid serving as an initial raw material and trishydroxymethyl aminomethane to obtain N-trishydroxymethyl-adamantane carboxamide; and 2) reacting with the molybdenum-containing polyoxometalate to obtain the hybrid compound. By the invention, the molybdenum-containing polyoxometalate and the adamantine are connected through the covalent bond for the first time; and the synthesis method is simple and feasible, reaction conditions are easy to realize, purification is simple, and the yield is high. The hybrid molecule has potential application value in the aspects of medicines, lubricants, surfactants, catalysts and the like.

Description

technical field [0001] The invention relates to the preparation of a hybrid compound of polyoxometalate, in particular to an adamantane hybrid compound containing molybdenum polyoxometalate and a preparation method thereof. Background technique [0002] Polyoxometalates (Polyoxometalates, POMs, referred to as polyacids) are a class of unimolecular clusters formed by the connection of early transition metal atoms through oxygen coordination bridges, of which vanadium, molybdenum, tungsten and other elements are the main representatives. . The size of polyoxometalates is about 0.5nm-5nm, with rich chemical composition and various topological structures, and exhibits excellent properties in catalysis, medicine, and optical, electrical, and magnetic functional materials. With the development of modern synthesis technology and research methods, polyoxometallates with new structures emerge in endlessly, and new properties are constantly being discovered (see "Introduction to Hete...

Claims

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Application Information

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IPC IPC(8): C07F19/00
Inventor 王维杨洁胡敏标杨海宽于伟
Owner NANKAI UNIV
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