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Method for synthesizing disulfide compound

A synthesis method and a disulfide technology are applied in the field of disulfide synthesis, which can solve the problems of complicated operation, unreusable catalyst and high production cost, and achieve simple and safe operation, favorable for large-scale industrial production and low cost. Effect

Inactive Publication Date: 2009-12-30
LIAONING UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And the use of chloride and sodium pyrosulfate under the action of a phase transfer catalyst to obtain the Bundt salt, and then treat the Bundt salt with DMSO to obtain disulfide compounds. This type of method is cumbersome to operate, the catalyst cannot be reused, and the production cost is higher

Method used

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  • Method for synthesizing disulfide compound

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Experimental program
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Effect test

Embodiment 1

[0022] Add 12.7g (0.1mol) of benzyl chloride, 1.6g (0.05mol) of sulfur powder, 0.32g (0.004mol) of selenium powder, 18mL (1mol) of water, and Sodium 4g (0.05mol) and solvent DMF 400mL, continue to pass through carbon monoxide, then heat to 95 ° C and stir for 2 hours, after cooling to room temperature, switch carbon monoxide gas to air, stir for 0.5 to 1 hour, at this time the unreacted selenium is separated out, filtered, and the filtrate is collected, and water with an amount 3 times the volume of the filtrate is added to the filtrate, at this time, the product dissolved in the filtrate is separated out, filtered, washed with water, and dried in vacuum to obtain the target product. The product has a purity of 100% and a yield of 94% as measured by proton nuclear magnetic resonance spectroscopy. (calculated as dibenzyl disulfide).

Embodiment 2

[0024] Only change the raw material of halogenated hydrocarbon, test method and other conditions are with embodiment 1.

[0025] Halogenated hydrocarbon

Embodiment 3

[0027] Temperature of reaction, sulfur powder amount, the reaction times are as follows, and experimental method and other conditions are with embodiment 1, and yield is as follows:

[0028] sulfur

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Abstract

The invention relates to a method for synthesizing disulfide compound. The invention adopts the technical scheme as follows: using halogenated hydrocarbon and sulphur as materials, selenium as the catalyst, organic base or inorganic base as the auxiliary catalyst or without any auxiliary catalysts, leading in carbon monoxide gas into organic solvent, reacting for 1-24 hours at 20-100 DEG C under normal pressure with the presence of water, cooling to a room temperature, switching the carbon monoxide gas into air or oxygen to separate out unreacted selenium, filtering, collecting the filtrate, then adding water with a volume of 2-3 times of the filtrate, and separating out the product to obtain the disulfide compound. The method is realized under normal-pressure reaction, has little device investment, convenient and safe operation, low cost, environmental protection, low difficulty of the reaction process and favorable economical property, and has phase shift function.

Description

technical field [0001] The invention relates to the synthesis of disulfides, in particular to a method for synthesizing disulfide compounds by selenium-catalyzed reaction by using halogenated hydrocarbons and sulfur as raw materials, utilizing carbon monoxide and water. Background technique [0002] Disulfide compounds are a class of important synthetic intermediates, which have important applications in organic synthesis, especially in the synthesis of physiologically active compounds. At the same time, it can be used as photoinitiator, chemical auxiliary agent for medicine and rubber regeneration. Disulfide compounds can be synthesized by a variety of methods: mainly obtained by oxidative coupling of mercaptans. There are many such oxidants, such as: bromodimethylsulfur bromide, Br 2 / KHCO 3 solution, p-toluenesulfonyl chloride, and even some metal oxides Fe 2 o 3 , MnO 2 and I 2 etc. In addition, electrochemical oxidation is also an effective method. Although the m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07B45/00C07C321/20C07C321/18C07C323/07C07C319/22C07D307/38B01J27/057B01J23/04B01J27/232B01J27/236B01J31/04B01J31/02
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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