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Ethyl trifluoroacetate preparation method

A technology of ethyl trifluoroacetate and trifluoroacetic acid, which is applied in the field of preparation of ethyl trifluoroacetate, can solve the problems of not being able to directly obtain pure ethyl trifluoroacetate, and achieve easy industrial production, mild conditions and low raw material cost low effect

Active Publication Date: 2017-02-22
NANTONG BAOKAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since ethanol and ethyl trifluoroacetate will form an azeotrope, this process cannot directly obtain pure ethyl trifluoroacetate, and it also needs to go through the process of washing to remove ethanol and drying, and finally the yield of the overall finished product is only 90%. , the washing process will also produce a large amount of waste water, forming a new environmental protection problem

Method used

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  • Ethyl trifluoroacetate preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0019] The 2000L reactor is equipped with a 12-meter rectification tower, which is divided into a 6-meter extraction section, a 6-meter rectification section, and a 16-meter distillation section. 2 enamel condenser. A solid superacid is used as a catalyst.

[0020] Add 500Kg ethyl trifluoroacetate to the reaction kettle in advance, and then raise the temperature to reflux. After the components in the rectification tower are stable, start to add trifluoroacetic acid from the top of the extraction section at a rate of 100kg / h. , began to add absolute ethanol to the reactor at a rate of 40kg / h, and after 10 minutes of total reflux, the temperature at the top of the column was stable at 61°C, and began to extract ethyl trifluoroacetate at a rate of 125kg / h.

[0021] After 10 hours, the feed and extraction were stopped. After the reactor cooled down, the materials in the reactor were left to stand for stratification, and the organic layer in the reactor and the obtained pure ethyl...

Embodiment 2

[0023] The 2000L reactor is equipped with a rectification tower with a diameter of 200mm and a height of 12 meters, which is divided into a 6-meter extraction section, a 6-meter distillation section, and a 16-meter distillation section. 2 enamel condenser. Concentrated sulfuric acid is used as catalyst.

[0024] Under cooling conditions, slowly add 150kg of concentrated sulfuric acid to 1000kg of trifluoroacetic acid in advance, mix well and pump the trifluoroacetic acid into the high level tank. Add 500Kg ethyl trifluoroacetate in the reaction kettle, then raise the temperature and reflux, after the components in the rectifying tower are stabilized, start to add trifluoroacetic acid from the top of the extraction section at a rate of 115kg / h, while adding trifluoroacetic acid, Start to add dehydrated ethanol to the reaction kettle at a rate of 40kg / h. After 10 minutes of total reflux, the temperature at the top of the column is stable at 61°C, and start to extract ethyl trif...

Embodiment 3

[0027] 2000L reactor, equipped with a rectification tower with a diameter of 200mm and a height of 15 meters, which is divided into a 7-meter extraction section, an 8-meter rectification section, and a 20m 2 enamel condenser. Concentrated sulfuric acid is used as catalyst.

[0028] Under cooling conditions, slowly add 150kg of concentrated sulfuric acid to 1000kg of trifluoroacetic acid in advance, mix well and pump the trifluoroacetic acid into the high level tank. Add 400Kg of trifluoroacetic acid, 80kg of concentrated sulfuric acid, and 161.5kg of absolute ethanol into the reaction kettle, and then raise the temperature and reflux for 30 minutes. After the components in the rectification tower are stabilized, start adding three Fluoroacetic acid, while adding trifluoroacetic acid, began to add absolute ethanol to the reaction kettle at a rate of 40kg / h. After 10 minutes of total reflux, the temperature at the top of the tower was stable at 61°C, and began to extract triflu...

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Abstract

The invention discloses an ethyl trifluoroacetate preparation method which includes the steps: pre-adding an appropriate amount of trifluoroacetic acid, ethyl alcohol and concentrated sulfuric acid into a reaction kettle with a rectifying tower according to prescribed proportion, or directly adding a certain amount of ethyl trifluoroacetate; rising temperature, performing backflow, and adding the ethyl alcohol and the trifluoroacetic acid of predetermined proportion from the top ends of a tower kettle and an extraction section of the rectifying tower respectively after proportion of various components in the rectifying tower is balanced and stabilized; directly collecting products at the top end of the rectifying tower after the products are purified to obtain the ethyl trifluoroacetate. According to the preparation method, solid super-acid or concentrated sulfuric acid serves as a catalyst, the trifluoroacetic acid and the ethyl alcohol are continuously fed, water in the tower kettle is regularly and quantitatively removed, continuous generation is achieved, production capacity is improved, reaction yield can reach 99%, and product purity can reach 99.9%.

Description

technical field [0001] The invention belongs to the field of organic intermediates, in particular to a preparation method of ethyl trifluoroacetate. Background technique [0002] Ethyl trifluoroacetate is an important organic intermediate widely used in pesticide, pharmaceutical and chemical industries. In the field of pesticides, highly active insecticides, acaricides, ovicides, and herbicides can be synthesized. In the field of medicine, it can be used as a medicine intermediate to prepare efavirenz, a medicine for treating AIDS. [0003] Its synthesis is mainly derived from the esterification of trifluoroacetic acid and ethanol. The traditional synthesis process is to cool the trifluoroacetic acid, then add absolute ethanol under stirring, the reaction is exothermic, and after the exotherm stops, slowly add concentrated sulfuric acid. After heating to reflux for half an hour, carry out fractional distillation and collect fractions at 62-64°C to obtain ethyl trifluoroac...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C67/54C07C69/63
CPCC07C67/08C07C67/54C07C69/63
Inventor 李华新闫宗刚葛繁龙吴盛均
Owner NANTONG BAOKAI CHEM
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