Synthesis method of 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 problems such as unsuitable drying of crude products, meet the requirements of simplified equipment and simple operation process , the effect of improving purity and yield

Active Publication Date: 2015-06-17
TRUST CROP PROTECTION TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the publication (announcement) number CN101397249, the reaction uses dehydrated alcohol to synthesize, and every batch of D72 ion resin synthesis needs to be filtered, and there is an inappropriate place in the drying aspect of the crude product

Method used

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  • Synthesis method of ethyl trifluoroacetate

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preparation example Construction

[0021] A synthetic method for ethyl trifluoroacetate, comprising the following steps:

[0022] Step 1. Use trifluoroacetic acid and ethanol as raw materials, use strong acidic cation exchange resin as catalyst, add ethanol dropwise at 40~50°C and normal pressure and keep it for 20 minutes, heat up and reflux to separate the mixture of water and ethanol to complete the reaction ;

[0023] Step 2, collecting the mixture of crude product ethanol and ethyl trifluoroacetate;

[0024] Step 3: After receiving the mixture in step 2, continue to use the catalyst and ethanol at the bottom of the kettle; add a small amount of water to wash the collected crude product with ethanol, and layer it to obtain a qualified product trifluoroacetic acid with a content of more than 99.5% and a moisture content of less than 0.1%. Ethyl ester, the yield is more than 95%;

[0025] Step 4, reflux to separate the dilute ethanol and merge with the dilute alcohol washed in step 3, and rectify to obtain ...

Embodiment 1

[0029] Put 200g of catalyst D72 resin and 360g of trifluoroacetic acid into a 1000ml single-necked bottle, stir to raise the temperature to 40°C, add 300g of absolute ethanol dropwise, and keep the temperature at 50°C to complete the dropwise addition. Stir for 20 minutes, heat up and reflux to separate about 60 g of the mixture of water and ethanol, start distillation, collect the product and the mixture of ethanol and water, and stop heating when the gas phase temperature reaches 65°C and there is no distillate. 510 g of crude product were collected. The distilled crude product, containing 15% alcohol, is washed once by adding 20% ​​of the weight of water, and the liquid is separated. The crude product of about 95% in the lower layer can be washed twice according to this method to obtain ethyl trifluoroacetate with a purity of 99.5%. Slowly heat up the product to 50-60°C for dehydration, and obtain 415g of a product with a moisture content of less than 0.1%.

[0030] The se...

Embodiment 2

[0032] The reaction kettle of Example 1 was drained of the jacket steam of the reaction kettle, the temperature of the circulating water was lowered to 20° C., and the second batch of materials was added: 360 g of trifluoroacetic acid, 200 g of absolute ethanol was added dropwise, and the same operation as before was collected to collect the product. The catalyst and undistilled ethanol are reused.

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Abstract

A synthesis method of ethyl trifluoroacetate comprises the steps: with trifluoroacetic acid and ethanol as raw materials, with strong acidic cation exchange resin as a catalyst, at a temperature of 40-50 DEG C and at normal pressure, dropwise adding ethanol and maintaining for 20 minutes, heating up and refluxing to separate out a water and ethanol mixture, and making the reaction completed; after collecting a crude product, continuing to use the kettle bottom catalyst and ethanol; adding water to the collected crude product to wash ethanol, stratifying to obtain ethyl trifluoroacetate with the yield of more than 95%; and refluxing to separate out dilute ethanol, and rectifying to obtain 95% ethanol for repeated use. The method omits a drying tower and a filtration device used in a conventional process; ethanol recovered from the reaction can be repeatedly used after treatment, the production cost is effectively reduced, and the method has the advantages of simple operation process, environmental protection, energy saving and no pollution; because price difference between trifluoroacetic acid and ethyl trifluoroacetate is not large, requirements on the product yield and cost are higher; and the method is complete and standardized in process, convenient to operate and suitable for industrialized production, and can effectively improve the purity and yield of the product.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, in particular to a method for synthesizing ethyl trifluoroacetate. Background technique [0002] Ethyl trifluoroacetate is an important organic chemical raw material, which can be used to synthesize organic fluorine compounds such as ethyl trifluoroacetoacetate, trifluoroacetylacetone, etc. It can also be used as an intermediate of medicine and pesticide, and organic synthesis. Ethyl trifluoroacetate is obtained by the esterification of trifluoroacetic acid and ethanol. Because the price of trifluoroacetic acid is higher, it is necessary to increase the reaction yield. [0003] "Hebei Chemical Industry" Vol. 35 No. 6 P24~25 is based on trifluoroacetic acid and absolute ethanol as the main raw materials, using p-toluenesulfonic acid as the catalyst, heating to reflux, and fractionally distilling the crude product. The crude product is passed through anhydrous calcium chloride Dry with anhydrous...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/63C07C67/08
CPCC07C67/08C07C69/63
Inventor 车鈜席亚男王成秀钟奇军
Owner TRUST CROP PROTECTION TECH CO LTD
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