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Method for preparing binuclear tricarbonyl chrominium complex

A technology of chromium tricarbonyl and complexes, which is applied in the field of preparation of binuclear chromium tricarbonyl complexes, can solve the problems of large loss and limitations in the research and application of binuclear chromium tricarbonyl complexes, and achieve high stability and excellent reaction conditions Gentle, highly operable effect

Inactive Publication Date: 2007-06-27
EAST CHINA UNIV OF SCI & TECH
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Problems solved by technology

Because the amount of binuclear products that can be obtained by this method is very small, the extraction process is often accompanied by a large loss, thus making the research and application of binuclear chromium tricarbonyl complexes greatly restricted.

Method used

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  • Method for preparing binuclear tricarbonyl chrominium complex

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preparation Embodiment 1

[0010] by η 6 -Vinyl carbazole chromium tricarbonyl as raw material (see Figure 1 for the crystal structure), using dioxane as a medium, prepare its saturated solution at 25 °C, use standard Schlenk technology for deoxidation treatment, magnetic stirring, at 75 °C Sealed and heated for 30 hours. The product system is precipitated with petroleum ether and dried in vacuum to obtain binuclear η 6 - Vinylcarbazole chromium tricarbonyl. The resulting product is crystallized using a mixed solvent of dichloromethane and n-hexane at low temperature to obtain a binuclear η 6 - A single crystal of vinylcarbazole chromium tricarbonyl, as shown in Figure 2.

preparation Embodiment 2

[0012] According to the method of Example 1, a mixed solvent of dioxane and n-butyl ether with a volume ratio of 1:1 was used as the medium, and its saturated solution was prepared at 25°C, sealed and heated at 120°C for 45 hours, and obtained by η 6 - Ethylcarbazole chromium tricarbonyl to give binuclear η 6 -Ethylcarbazole chromium tricarbonyl.

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Abstract

This invention has disclosed a manufacturing method to binuclear tricarbonyl chromium complex. It adopts single-nuclear eta<6> tricarbonyl chromium complex as raw materials, one kind or many kinds of mixture of dioxane, tetrahydrofurans, butylether as medium, deoxidize with standard Schlenk technology, under the condition of mixing, when the temperature is 50 DEG C to 150 DEG C, sealed heating 20 to 40 hours, precipitate reaction products with petroleum ether, get binuclear tricarbonyl chromium complex finally. Production ratio of binuclear tricarbonyl chromium complex is up to 30 percent.

Description

technical field [0001] The present invention relates to a kind of preparation method of the chelate compound of the compound containing>C=O group, more specifically relate to a kind of preparation of the dinuclear tricarbonyl chromium complex with carbazole and its derivatives as organic ligands method. Background technique [0002] The η6 aromatic hydrocarbon chromium tricarbonyl complex has a typical D-π-A structure due to its chromium tricarbonyl group can interact with the delocalized π electrons of the aromatic ring, and has good applications in the fields of optoelectronics, molecular design, and catalysis. Application prospects. Especially the binuclear chromium tricarbonyl complex, due to the introduction of two chromium tricarbonyl groups with strong electron-withdrawing ability into the organic ligand molecule, an electronic resonance structure is formed inside the molecule, making it compatible with the mononuclear complex Compared with the nature, there has ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F11/00
Inventor 田晓慧施维车延超张平陈辉
Owner EAST CHINA UNIV OF SCI & TECH
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