Method for preparing ethyl bromodifluoroacetate

A technology of ethyl difluorobromoacetate and ethyl difluoroacetate is applied in the field of preparation of chemical reagents, can solve the problems of dangerous handling, industrial difficulty in obtaining ethyl difluorobromoacetate, increased production cost, etc., and achieves low equipment investment. , the effect of simple post-treatment and mild reaction conditions

Inactive Publication Date: 2018-01-12
盐城顺恒化工有限公司
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Problems solved by technology

[0003] Although there are many synthetic methods for ethyl difluorobromoacetate, some raw materials for the synthesis of ethyl difluorobromoacetate are either difficult to obtain in industry, or are very dangerous to handle, requiring very special instruments and devices, so increased production costs

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Embodiment Construction

[0022] The best mode for carrying out the present invention is described below.

[0023] A kind of preparation method of ethyl difluorobromoacetate of present embodiment 1, take trichloroethylene as raw material, comprises the steps:

[0024] S1. Put trichlorethylene in the reactor, add the composite catalyst, stir evenly, heat to 70-100°C, turn on the 150W high-pressure mercury lamp, and pass through the sulfuric acid dried at a speed of 500ml / min under vigorous stirring. Air, keep it for 18-24h, carry out atmospheric distillation processing on the resultant, collect 105-108°C fractions, and obtain the product dichloroacetyl chloride; the composite catalyst is manganese dioxide, triphenylphosphine and ammonium chloride, and the composite catalyst The weight ratio to trichlorethylene is 0.1-1.0:100.

[0025] S2. Put diethylamine and toluene into the reaction kettle in turn at room temperature, stir, control the temperature below 10°C, and add dichloroacetyl chloride dropwise ...

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Abstract

The invention provides a method for preparing ethyl bromodifluoroacetate and relates to a preparation method of a chemical reagent. The method takes trichloro ethylene as a raw material, and comprisesthe following steps: under the action of ultraviolet light of a catalytic medium, an oxidation reaction happens between trichloro ethylene and oxygen in a reactor to synthesize dichloracetyl chloride; an amination reaction happens between dichloracetyl chloride and diethylamine under the action of a catalyst to synthesize dichloroacetyl diethylamine; a fluorination reaction happens between dichloroacetyl diethylamine and anhydrous potassium fluoride under the action of a solvent and a phase transfer catalyst to synthesize difluoroacetyl diethylacetamide; difluoroacetyl diethylacetamide is esterified to synthesize ethyl difluoroacetate; and by taking cupric bromide as a brominating agent, ethyl difluoroacetate is bromized to prepare the end product (ethyl bromodifluoroacetate). The methodhas the characteristics that the equipment investment is low, reaction conditions are mild, the method is safely implemented at normal pressure, and after-treatment is simple.

Description

technical field [0001] The invention relates to a preparation method of chemical reagents, in particular to a preparation method of ethyl difluorobromoacetate. Background technique [0002] The synthesis of ethyl difluorobromoacetate is a relatively classic intermediate synthesis reaction, and the research on its synthesis process is also very rich. The most commonly used is to prepare alcohols with bromodifluoroacetyl halides (acyl fluorides, acid chlorides or acid bromides). These bromodifluoroacetyl halides are generally prepared by 1,1-difluorotetrahalogenated ethane such as CF 2 BrCFClBr, CF 2 BrClBr 2 、CF 2 BrCBr 3 、CF 2 BrCF 2 Br is produced by oxidation with sulfuric acid in the presence of metal salt catalysts, especially in the presence of mercury salt catalysts. [0003] Although there are many synthetic methods for ethyl difluorobromoacetate, some raw materials for the synthesis of ethyl difluorobromoacetate are either difficult to obtain in industry, or a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/307C07C69/63
Inventor 田其雄刘昌奎李加华刘龙龙
Owner 盐城顺恒化工有限公司
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