Catalyst for synthesis of difluoro ethyl acetoacetate and preparation method thereof

Abstract

The invention discloses a catalyst for synthesis of difluoro ethyl acetoacetate and a preparation method thereof, the catalyst comprises the following components by weight: 0.5-1 part of sodium bromide, 1- 4 parts of NiCl2, 2-5 parts of magnesium oxide, 0.8-2 parts of potassium carbonate, 5 -10 parts of activated carbon, 1-5 parts of polycarbonate, 0.5-1 part of zirconium dioxide, 5-10 parts of ethanol, 1-5 parts of polyacrylamide, and 8-15 parts of deionized water; the preparation method is as follows: 1, the magnesium oxide, the potassium carbonate and the polycarbonate are stirred and mixed at certain temperature to obtain a mixture I; 2, the zirconium oxide, the sodium bromide, the NiCl2, the polyacrylamide and the deionized water are added into the mixture I, and after stirring evenly, heating for reaction and cooling to room temperature, a mixture II is obtained; 3, the activated carbon and the ethanol are added into the mixture II, and after heating for reaction under certain vacuum degree, and cooling and filtering, a solid precipitate is obtained; and 4, finally the solid precipitate is dried, sintered, cooled, cleaned, and dried.

Description

technical field [0001] The invention provides a catalyst for synthesizing ethyl difluoroacetoacetate and a preparation method thereof, belonging to the field of chemical catalyst preparation. Background technique [0002] Ethyl difluoroacetoacetate is an important pharmaceutical and chemical intermediate. The application of its synthesis process has very important industrial application value. At present, relevant research reports on its synthesis method and application have been carried out at home and abroad, but the current synthesis of difluoroacetoacetate Ethyl fluoroacetoacetate is mainly obtained by reacting ethyl difluoroacetate and ethyl acetate to obtain ethyl difluoroacetoacetate, wherein sodium ethoxide is used as a catalyst, and the reaction time of this method generally takes 4-5 hours, and the reaction cycle is relatively short. long, the product yield can reach about 70%, and the ethanol that exists in the system after the reaction needs to be removed by azeo...

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Problems solved by technology

[0002] Ethyl difluoroacetoacetate is an important pharmaceutical and chemical intermediate. The application of its synthesis process has very important industrial application value. At present, relevant research reports on its synthesis method and application have been carried out at home and abroad, but the current synthesis of difluoroacetoacetate Ethyl fluoroacetoacetate is mainly obtained by reacting ethyl difluoroacetate and ethyl acetate to obtain ethyl difluoroacetoacetate, wherein sodium ethoxide is used as a catalyst, and the reaction time of this method generally takes 4-5 hours, and the reaction cycle is relatively short. long, the product yield can reach about 70%, and the ethanol that exists in the system after the reaction needs to be removed by azeotropy, which brings inconvenience to industrialized production. At the same time, the recovered ethanol needs to be processed, which not only increases the production cost, At the same time, it also brings safety hazards to large-scale industrial production.

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