Method for synthesizing ethyl trifluoroacetate

A technology of ethyl trifluoroacetate and a synthesis method, which is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problem that potassium hydrogen fluoride solid cannot be handled, trifluoroacetyl fluoride raw material is rare and unsuitable Industrial production and other problems, to achieve the effect of low overall cost control, thorough response, and simple equipment requirements

Inactive Publication Date: 2018-12-07
山东沾化永浩医药科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Then this method uses acidic cation exchange resin as catalyst. Although it can be recycled after treatment, the activity will drop significantly every time it is used. New cation exchange resin must be added to achieve the desired esterification effect.
[0007] In addition, trifluoroacetyl fluoride reacts with ethanol and potassium fluoride to prepare ethyl trifluoroacetate. This method has rare raw materials for trifluoroacetyl fluoride, and the gas is dangerous. It is not suitable for industrial production and produces a large amount of potassium bifluoride solids that cannot be handled.

Method used

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  • Method for synthesizing ethyl trifluoroacetate
  • Method for synthesizing ethyl trifluoroacetate
  • Method for synthesizing ethyl trifluoroacetate

Examples

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example 1

[0022] A kind of synthetic method of ethyl trifluoroacetate of example 1

[0023] Throw 100 grams (0.877mol) of trifluoroacetic acid, 42.5 grams (0.922mol) of absolute ethanol, in a 500 ml three-necked flask, add 5.5 grams (4.4mmol) of solid acid catalyst, the number of moles per gram of solid acid catalyst is 0.8mmol) , start stirring at 20°C and keep it warm for 8 hours, take a sample test, the trifluoroacetic acid is 0.48%, stop stirring, use a separatory funnel to remove the lower part of the water, transfer the upper material layer into a three-necked flask, put in 2.2 grams of solid acid catalyst, start stirring Continue to react for 1 hour at 20°C, take a sample for detection, 0.08% trifluoroacetic acid, after the reaction is complete, pour the feed liquid into another 500 ml three-necked flask, the flask is equipped with a 40 cm 24# caliber rectification column (glass spring packing), Start stirring, heat up and rectify; receive the distillate at 60-62°C to obtain 122....

example 2

[0024] A kind of synthetic method of ethyl trifluoroacetate of example 2

[0025] Throw 100 grams (0.877 mol) of trifluoroacetic acid and 42.5 grams (0.922 mol) of absolute ethanol into a 500 ml three-necked flask, add 5.5 grams of solid acid catalyst, start stirring at 30 ° C for 4 hours, and take samples for detection. Acetic acid 0.42% (required to be less than 0.5%), stop stirring, pour into a separatory funnel to separate the lower part of the water, transfer the upper material layer into a three-necked flask, put in 2.2 grams of solid acid catalyst, start stirring at 20 °C and continue the reaction for 1 hour, sampling and testing , trifluoroacetic acid 0.05% (required to be less than 0.1%), after completion of the reaction, feed liquid is poured in another 500 milliliters there-necked flask, the rectifying column (glass spring packing) of 40 centimeters of 24# calibers of flask assembly, start stirring, Heating rectification; receive the distillate at 60-62° C. to obtai...

example 3

[0026] A kind of synthetic method of ethyl trifluoroacetate of example 3

[0027] Throw 100 grams (0.877 mol) of trifluoroacetic acid and 42.5 grams (0.922 mol) of absolute ethanol into a 500 ml three-necked flask, add 8.0 grams of solid acid catalyst, start stirring at 30 ° C for 2 hours, and take samples for detection. Acetic acid 0.45% (required to be less than 0.5%), stop stirring, pour into a separatory funnel to separate the lower part of the water, transfer the upper material layer into a three-necked flask, put in 2.2 grams of solid acid catalyst, start stirring at 20 °C and continue the reaction for 1 hour, sampling and testing , trifluoroacetic acid 0.04% (required to be less than 0.1%), after completion of the reaction, feed liquid is poured in another 500 milliliters there-necked flask, and the rectifying column (glass spring packing) of 40 centimeters of 24# calibers of flask assembly, starts stirring, Heating rectification; receiving the distillate at 60-62° C. t...

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Abstract

The invention relates to a method for synthesizing ethyl trifluoroacetate. Raw materials in the method for synthesizing ethyl trifluoroacetate include trifluoroacetic acid and anhydrous ethanol, and acatalyst is a solid acid catalyst. The method provided by the invention is simple in process, low in equipment requirement, and thorough in reaction, with the purity of 99.5% or above, and the molaryield of 98.0% or above. The solid acid catalyst can be recycled after being dried, and the activity is not significantly decreased, so that the using amount of the catalyst is small. The overall costof the method provided by the invention is controlled to be relatively low, thus being suitable for industrial production.

Description

technical field [0001] The invention relates to a method for synthesizing ethyl trifluoroacetate, which belongs to the technical field of chemical synthesis. Background technique [0002] Ethyl trifluoroacetate, F 3 CCOOCH 2 CH 3 It is an important organic chemical raw material, mainly used in the synthesis of organic fluorine compounds and the preparation of industrial chemicals such as pesticides, medicines, dyes, and liquid crystals, and has a wide range of uses. In medicine, it is used to manufacture anti-inflammatory drugs for treating rheumatoid arthritis and osteoarthritis, and anti-tumor drugs for treating colorectal cancer. Pesticides are used in the manufacture of cell division inhibitors for cotton and peanuts to eliminate grasses, grasses, and broad-leaved weeds. The prospect of development and application is broad, and the market is in short supply. [0003] In the prior art, the synthetic method of ethyl trifluoroacetate mainly contains following several. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/63C07C67/08
CPCC07C67/08C07C69/63Y02P20/584
Inventor 倪政
Owner 山东沾化永浩医药科技有限公司
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