Method for preparing bis(4-tert-butyl benzyl)sulfide product

Abstract

The invention relates to a method for preparing a bis(4-tert-butyl benzyl)sulfide product, belonging to the technical field of preparation of medical intermediate compounds and polymer antioxidants. The method comprises the following step: in the presence of both an emulsifier and a phase-transfer catalyst, reacting 4-tert-butyl benzyl chloride and a sodium sulfide water solution used as raw materials in an organic solvent-water system, wherein the proportioning of the raw materials is as follows: the mol ratio of the 4-tert-butyl benzyl chloride to the sodium sulfide is 1:(0.5-0.9); the mass ratio of the 4-tert-butyl benzyl chloride to the organic solvent is 1:(0.8-1.6); the mass ratio of the 4-tert-butyl benzyl chloride to the emulsifier is 1:(0.008-0.033); the mass ratio of the 4-tert-butyl benzyl chloride to the phase-transfer catalyst is 1:(0.008-0.033); the reaction temperature in the reaction process is 50-70 DEG C; and the reaction time is 150-240 minutes. Thus, high raw material conversion rate and product yield are achieved.

Description

technical field [0001] The invention relates to a method for preparing an organic compound bisbenzyl sulfide product, which belongs to the technical field of preparation of pharmaceutical intermediates and polymer antioxidants, and specifically relates to the preparation technology of a compound bis(4-tert-butylbenzyl) sulfide product , the product structure is as follows: . [0002] Background technique [0003] Dibenzyl sulfide and its oxidation products are important organic synthesis intermediates, widely used in the production of pharmaceuticals, polymer synthetic materials and other fine chemical products raw materials, the oxidized derivatives of dibenzyl sulfide dibenzyl Sulfoxide is an acid corrosion inhibitor of iron and dibenzylsulfone is a very effective bacterial growth inhibitor. Bis(4-tert-butylbenzyl)sulfide is oxidized into bis(4-tert-butylbenzyl)sulfone under the action of hydrogen peroxide, which is an important pharmaceutical intermediate, and bis(4-t...

AI Technical Summary

Problems solved by technology

Its shortcoming is that the reaction system that ethanol and sodium sulfide is formed, the reaction solution that forms finally under reaction condition is brownish yellow, seriously pollutes the color and luster of target product, brings great difficulty to the refinement and purification of product, has increased greatly Production cost; In addition, repeatedly extract the product in the ethanol reaction mixture with ether, even so also can have a small part of product to remain in the ethanol mother liquor and influence the final yield of product, make industrial production process become very complicated as a result, produce Increased costs

Its disadvantage is that the reaction system composed of ethanol and sodium sulfide, the reaction solution finally formed under the reaction conditions is brownish yellow, seriously pollutes the color of the target product, and brings great difficulties to the recrystallization, refining and decolorization of the product, greatly Increased production cost; In addition, extracting the product in the ethanol reaction mixture with chloroform inevitably affects the final yield of the product, and the industrial production process becomes very complicated, and the production cost increases

Its disadvantage is that the reaction system composed of ethanol and sodium sulfide, the reaction solution finally formed under the reaction conditions is yellow, which seriously pollutes the color of the target product, brings great difficulties to the recrystallization, refining and decolorization of the product, and greatly increases cost of production

The disadvantage of this technology is that the organic layer is separated after the reaction, and the water layer is extracted twice with toluene, the organic layer is combined, the toluene solvent is evaporated after drying, and the product is obtained after recrystallization with ethanol. The production process is more complicated and vulcanized. The amount of sodium raw material is large, and the final product yield is low

The disadvantage is that the amount of sodium sulfide raw material is relatively large, and the final product yield is low