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Diselenide compound synthesis method

A synthesis method and technology of diselenide, applied in the direction of organic chemistry and the like, can solve the problems of complex operation, low yield, many steps, etc., and achieve the effects of high reaction selectivity, low equipment investment and simple raw materials

Inactive Publication Date: 2012-07-25
LIAONING UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantages of these methods are that there are many steps, complex operation, low yield, and direct utilization of hydrogen selenide gas

Method used

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  • Diselenide compound synthesis method

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Experimental program
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Effect test

Embodiment 1

[0021] Add 12.7g (0.1mol) of benzyl chloride, 4g (0.05mol) of selenium powder, 18mL (1mol) of water, 4g (0.05mol) of sodium acetate and 400mL of solvent DMF into a 1000mL three-necked flask equipped with a stirring bar and a condenser , continue to feed pure carbon monoxide gas, then heat to 95 ° C and stir for 2 hours, after cooling to room temperature, switch carbon monoxide to air or oxygen, and stir for 0.5 to 1 hour. At this time, unreacted selenium is precipitated. Filter and collect the filtrate. Add water of 3 times the volume of the filtrate to the filtrate, at this time the product dissolved in the filtrate is precipitated, filtered, washed with water, and dried in vacuum to obtain the target product. The product has a purity of 100% and a yield of 98% as measured by proton nuclear magnetic resonance spectroscopy. (as dibenzyl diselenide).

Embodiment 2

[0023] Only change the raw material of halogenated hydrocarbon, experimental method and other conditions are the same as embodiment 1.

[0024] Halogenated hydrocarbons

Embodiment 3

[0026] Reaction temperature, selenium amount, reaction time are as follows, and experimental method and other conditions are with embodiment 1, and yield is as follows:

[0027] Selenium

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Abstract

The invention relates to a diselenide compound synthesis method and the adopted technical proposal comprises the following steps: adopting halogenated hydrocarbon and selenium as raw materials and organic base or inorganic base as cocatalyst or no cocatalyst, continuously injecting carbon dioxide gas in organic solvent to react in the present of water under the temperature of 20-100 DEG C at normal pressure for 1-24h, cooling to the room temperature, switching carbon dioxide to air or oxygen to precipitate unreacted selenium, filtrating to collect filtrate, then adding 2-3 times of water, precipitating products and finally obtaining the diselenide compound by filtration. The method invention is normal press reaction with low cost, environmentally friend, low reaction process difficulty, convenient operation and easy following separation of products and catalyst.

Description

technical field [0001] The invention relates to the synthesis of diselenide, in particular to a method for synthesizing diselenide through self-catalyzed reaction of selenium by using halogenated hydrocarbon and selenium as raw materials, utilizing carbon monoxide and water. Background technique [0002] Diselenide is an important organic synthesis reagent and synthetic intermediate. Such as: the application of dibenzyl diselenide in the synthesis of natural products [J.Org.Chem., 1977, 7, 1228-1230]; the practical application is very wide, and it is used in the solid phase of dibenzyl diselenide in photoconductive materials In terms of separation [Document: US3994791; US4013530; GB15086683]; in cancer research, inhibiting carcinogenesis [Cancer Research, 1997, 21, 4757-4764]. The conventional method for synthesizing diselenides at present has [J.Am.Chem.Soc., 1975,97,5434-5436] that chlorinated hydrocarbons react with Grignard reagents; aromatic aldehydes directly react wi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C391/00C07C391/02C07D307/10
Inventor 刘晓智刁海倩于强张荷新李春荣龙慎杰毛颖
Owner LIAONING UNIVERSITY
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