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Processing technique of ethyl difluoroacetate

A technology of ethyl difluoroacetate and production process, applied in the field of production technology of ethyl difluoroacetate, can solve the problems of low total yield, equipment corrosion, long process flow, etc., and achieves improved production yield and industrialized production. , the effect of increasing the reaction rate

Inactive Publication Date: 2012-01-11
RUGAO JINLING CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the disadvantages of this process are: the synthesis of difluoroacetic acid and esters by potassium fluoride fluorination has problems such as long process flow, low total yield, and serious equipment corrosion.

Method used

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  • Processing technique of ethyl difluoroacetate
  • Processing technique of ethyl difluoroacetate
  • Processing technique of ethyl difluoroacetate

Examples

Experimental program
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Effect test

example 1

[0028] In a 1000ml reaction bottle, put 80g of diethylamine and 400ml of toluene respectively, lower the temperature, add 138g of dichloroacetyl chloride dropwise under 10°C for 1 hour, the dropwise addition is completed, keep the reaction for 2 hours, filter, and the filtrate is decompressed to recover toluene, reduce 160g of dichloroacetyldiethylamine was collected by pressure distillation at 95-110°C / 20mmHg. Yield: 93.1%.

[0029] Put 125g of dichloroacetyldiethylamine, 110g of anhydrous potassium fluoride, 5g of catalyst tetrabutylammonium bromide, and 230g of solvent sulfolane into a 500ml reaction bottle, start stirring, heat up, and keep warm at 145-150°C for 6 hours , after the reaction was completed, it was lowered to room temperature, filtered, and the filtrate was collected under reduced pressure at 120-130° C. / 20 mmHg fraction to obtain 86.7 g of difluoroacetyldiethylamine, yield: 84.5%.

[0030] Put 260g of difluoroacetyldiethylamine into a 500ml reaction bottle,...

example 2

[0032] In a 1000ml reaction bottle, put 80g of diethylamine and 400ml of toluene respectively, lower the temperature, add 138g of dichloroacetyl chloride dropwise under 10°C for 1 hour, the dropwise addition is completed, keep the reaction for 2 hours, filter, and the filtrate is decompressed to recover toluene, reduce 160g of dichloroacetyldiethylamine was collected by pressure distillation at 95-110°C / 20mmHg. Yield: 93.1%.

[0033] Put 125g of dichloroacetyldiethylamine, 100g of anhydrous potassium fluoride, 5g of catalyst tetrabutylammonium bromide, and 250g of recovered sulfolane into a 500ml reaction bottle, start stirring, raise the temperature, and keep warm at 145-150°C for 6 hours , after the reaction was completed, lowered to room temperature, filtered, and the filtrate was collected under reduced pressure at 120-130° C. / 20 mmHg fraction to obtain 85.3 g of difluoroacetyldiethylamine, yield: 83.1%.

[0034] Put 260g of difluoroacetyldiethylamine into a 500ml reactio...

example 3

[0036] In a 1000ml reaction bottle, put 80g of diethylamine and 400ml of toluene respectively, lower the temperature, add 138g of dichloroacetyl chloride dropwise under 10°C for 1 hour, the dropwise addition is completed, keep the reaction for 2 hours, filter, and the filtrate is decompressed to recover toluene, reduce 160g of dichloroacetyldiethylamine was collected by pressure distillation at 95-110°C / 20mmHg. Yield: 93.1%.

[0037]Put 125g of dichloroacetyldiethylamine, 120g of anhydrous potassium fluoride, 5g of catalyst tetrabutylammonium bromide, and 250g of recovered sulfolane into a 500ml reaction bottle, start stirring, heat up, and keep warm at 145-150°C for 6 hours , after the reaction was completed, lowered to room temperature, filtered, and the filtrate was collected under reduced pressure at 120-130° C. / 20 mmHg fraction to obtain 88.5 g of difluoroacetyldiethylamine, yield: 86.2%.

[0038] Put 260g of difluoroacetyldiethylamine into a 500ml reaction bottle, add 2...

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Abstract

The invention mainly discloses a processing technique of ethyl difluoroacetate, which mainly comprises the following steps of: preparing an intermediate product dichloroacetyl diethylamine through an amination process; carrying out fluorination with anhydrous potassium fluoride and the dichloroacetyl diethylamine as raw material under the action of a solvent and a phase transfer catalyst to prepare difluoro-acetyl diethylamine; and carrying out esterification to prepare the ethyl difluoroacetate. The processing technique of the ethyl difluoroacetate is characterized in that the solvent in the fluorination is sulfolane, and the esterification is a direction reaction of ethanol and the difluoro-acetyl diethylamine. The processing technique of the ethyl difluoroacetate specifically has the advantages of improving the final yield by changing the solvent during the fluorination and improving the production rate by carrying out the direct esterification after the fluorination.

Description

technical field [0001] The invention relates to a production process of ethyl difluoroacetate, in particular to a process for the production of ethyl difluoroacetate using a three-step process of amination, fluorination and esterification, which has fewer steps and high final product yield The advantages. Background technique [0002] EP0694523 discloses a preparation method of difluoroacetamide and its difluoroacetate. The method uses tetrafluoroethylene as a raw material, and tetrafluoroethylene is added with methanol in the presence of a catalyst to obtain methoxytetrafluoroethane (CH 3 OCF 2 CF 2 H), methoxytetrafluoroethane is catalytically cracked to obtain difluoroacetyl fluoride, and difluoroacetyl fluoride is absorbed by alcohol to obtain difluoroacetate. [0003] JP7242587 discloses a preparation method of difluoroacetic acid and its difluoroacetamide. Tetrafluoroethylene, diethylamine and water were reacted in an autoclave for 10 hours to obtain 79% N, N-diet...

Claims

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Application Information

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IPC IPC(8): C07C69/63C07C67/20
Inventor 赵祥领李桂萍石卫兵顾维新
Owner RUGAO JINLING CHEM
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