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Method for producing difluoroacetic acid ester

A technology of difluoroacetic acid ester and manufacturing method, which is applied to the preparation of carboxylic acid ester, the preparation of carboxylic acid halide, chemical instruments and methods, etc., can solve the problems of reducing the recovery rate, increasing the solubility, etc. Comprehensive yield, the effect of avoiding yield reduction

Inactive Publication Date: 2015-02-25
CENT GLASS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the methods described in these documents, in order to remove or detoxify the inert hydrogen fluoride that becomes the salt, washing with an aqueous solution is performed, but the fluorine-containing carboxylic acid ester has high hydrolyzability, and not only is decomposed by the addition of water, Moreover, the fluorine-containing carboxylic acid and alcohol produced with this reaction will increase the solubility of the ester itself in water, so the recovery rate is significantly reduced

Method used

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  • Method for producing difluoroacetic acid ester
  • Method for producing difluoroacetic acid ester
  • Method for producing difluoroacetic acid ester

Examples

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Embodiment

[0069] The present invention will be described below using examples, but the embodiments of the present invention are not limited thereto. In the examples, ethyl difluoroacetate (CHF 2 COOEt), ethanol (EtOH), difluoroacetic acid (CHF 2 COOH) and other organic components are measured by FID gas chromatography (GC), and the content of inorganic acids such as hydrogen fluoride is measured by ion chromatography (IC).

Synthetic example 1

[0071] Aluminum phosphate (Aluminum phosphate) produced by Aldrich was pelletized into pellets with a diameter of 5 mm x a length of 5 mm, and fired at 700° C. for 5 hours in a nitrogen stream to prepare an aluminum phosphate catalyst. 2200 cc of this was filled in a large gas phase reaction tube (made of stainless steel, inner diameter 43 mm x length 1800 mm) equipped with a vaporizer. While flowing nitrogen gas at a rate of 1000 cc / min, the reaction tube was heated by an external electric furnace. After the temperature of the catalyst reached 50° C., hydrogen fluoride (HF) was introduced at a maximum rate of 6 g / min through the vaporizer while monitoring so as not to generate sudden heat generation. In the state of circulating HF, slowly raise the temperature to 300°C, slowly increase the HF supply rate to 12g / min, and keep it at 300°C for 72 hours, after that, lower the set temperature of the heater, and the internal temperature reaches 250°C , stop the flow of HF, increas...

Synthetic example 2

[0073] Aluminum phosphate (Aluminum phosphate) produced by Aldrich was pelletized into pellets with a diameter of 5 mm x a length of 5 mm, and fired at 700° C. for 5 hours in a nitrogen stream to prepare an aluminum phosphate catalyst. 200 cc of this was filled in a small gas phase reaction tube (made of stainless steel, inner diameter 37 mm x length 500 mm) equipped with a vaporizer. While flowing nitrogen gas at a rate of 100 cc / min, the reaction tube was heated by an external electric furnace. After the temperature of the catalyst reached 50° C., hydrogen fluoride (HF) was introduced through the vaporizer at a maximum rate of 0.6 g / min while monitoring so as not to generate sudden heat generation. In the state of circulating HF, slowly raise the temperature to 300°C, slowly increase the HF supply rate to 1.2g / min, and keep it at 300°C for 72 hours, after that, lower the set temperature of the heater, and the internal temperature reaches 250 At ℃, stop the flow of HF, incre...

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Abstract

A production method of a difluoroacetic acid ester according to the present invention includes at least: a reaction step of obtaining a liquid by reaction of an alcohol represented by ROH with difluoroacetic acid fluoride (CHF 2 COF) in the presence of an amide compound of the following formula (1) or a sulfone compound of the following formula (2) as a hydrogen fluoride trapping agent; and a distillation step (A) of extracting a difluoroacetic acid ester represented by CHF 2 COOR by distillation of the reaction liquid obtained in the first step. In the present production method, there occurs no deterioration in the yield of the product due to the inherent generation of hydrogen fluoride as a by-product during the esterification reaction of difluoroacetic acid fluoride.

Description

technical field [0001] The present invention relates to a method for producing difluoroacetate used as a medicine and pesticide intermediate and a reaction reagent, and more particularly to a method for effectively removing by-product hydrogen fluoride (HF) in the reaction between difluoroacetyl fluoride and alcohol. Background technique [0002] As methods for producing difluoroacetic acid esters, the following methods have been proposed: (1) a method of reacting difluoroacetic acid with an alcohol, (2) a method of making 1-alkoxy-1,1,2,2-tetrafluoroethane , the method of reacting sulfuric acid and silicon dioxide (non-patent literature 1), (3) bubbling the reaction crude gas containing difluoroacetyl fluoride into a mixture of ethanol and triethylamine, followed by washing with water and extracting with dichloromethane, A method of obtaining ethyl difluoroacetate (Patent Document 1) and the like. [0003] In the esterification reaction between carboxylic acid fluoride and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/14C07C67/54C07C67/62C07C69/63
CPCC07C67/14C07C67/54C07C69/63
Inventor 冈本正宗高田直门井村英明
Owner CENT GLASS CO LTD
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