Synthesis method of 4,4'-thiobisbenzenethiol

Abstract

The invention discloses a synthesis method of 4,4'-thiobisbenzenethiol. The method comprises the following steps of: 1) esterfying, namely adding acetic anhydride into phenthiol serving as an initiative raw material dropwise for reacting, and laminating; 2) etherifying, namely adding a solvent, iodine and sulfur dichloride into an organic layer I obtained in the step 1) for reacting, laminating, decompressing an organic layer II and removing the solvent to obtain a yellow solid; 3) hydrolyzing, namely adding sodium hydroxide and the yellow solid into water for a warming reflux reaction, adding hydrochloric acid solution dropwise, and filtering to obtain a white solid; and 4) recrystallizing, namely recrystallizing the white solid with a recrystallizing solvent to obtain white crystalline 4,4'-thiobisbenzenethiol. The 4,4'-thiobisbenzenethiol synthesized by the method has the characteristics of simple process and high yield.

Description

The synthetic method of 4,4'-dimercaptodiphenyl sulfide technical field The present invention relates to a kind of synthetic method of 4,4'-dimercapto diphenyl sulfide. Background technique 4,4'-dimercapto diphenyl sulfide as shown in formula I is widely used in fine chemical intermediates such as medicine, pesticide and dyestuff. Formula I CN02114837.6 has reported that with diphenyl sulfide and chlorosulfonic acid as starting raw materials, 4,4'-dimercapto diphenyl sulfide is obtained through chlorosulfonation and zinc powder reduction; the required zinc powder consumption of this method Large, expensive, and the obtained product has many isomers and the content is not high. JP06032773 and JP04264064 reported the reaction of diphenyl sulfide and dichlorodisulfide, and the reduction of triphenylphosphine to prepare 4,4'-dimercapto diphenyl sulfide. This method also has many isomers, and triphenyl The high price of phosphine greatly limits its industrial production....

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Problems solved by technology

JP06032773 and JP04264064 reported the reaction of diphenyl sulfide and dichlorodisulfide, and the reduction of triphenylphosphine to prepare 4,4'-dimercapto diphenyl sulfide. This method also has many isomers, and triphenyl Phosphine is expensive and other deficiencies greatly limit its industrial production

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