Process for synthesizing 2, 3, 3, 3-tetrafluoropropionic acid

A synthesis method and technology of tetrafluoropropionic acid, applied in the directions of organic chemistry, amide preparation, etc., can solve the problems of increasing the difficulty and cost of waste liquid treatment in factories, many by-product impurities, difficult reaction control, etc., and achieve low price and rapid reaction. , Easy to operate effect

Active Publication Date: 2013-08-21
京山瑞生制药有限公司
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the main synthesis route of 2,3,3,3-tetrafluoropropionic acid is to replace propionic acid with fluorine. The disadvantage of this process is that the reaction is difficult to control, the by-products are many impurities, and it is not easy to purify, so the yield is not high.
[0006] N,N-diethyl-2,3,3,3-tetrafluoropropionamide is N,N-diethyl-1,1,2,3,3,3-hexafluoropropylamine after fluorine substitution reaction The by-products are difficult to degrade, which greatly inc

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 201 g (1.0 mol) of N,N-diethyl-2,3,3,3-tetrafluoropropionamide, 100 g of concentrated sulfuric acid (98%), 16 g of water, and 10.05 g of copper sulfate into the three-necked flask, and stir to raise the temperature The temperature was 120°C, and the reaction was carried out for 6 hours. TLC detected that the reaction was complete, and fractional distillation was started to obtain 140 g of the product with a GC content of 99.6% and a molar yield of 96%.

Embodiment 2

[0023] Add 201 grams (1.0mol) of N,N-diethyl-2,3,3,3-tetrafluoropropionamide, 2147 grams of 17% hydrochloric acid aqueous solution and 2.01 grams of copper chloride into the three-necked flask, stir and heat up to 40 ℃, reacted for 30 hours, TLC detected that the reaction was complete, and started fractional distillation to obtain 132 g of the product with a GC content of 99.2% and a molar yield of 91%.

Embodiment 3

[0025] Add 201 grams (1.0mol) of N,N-diethyl-2,3,3,3-tetrafluoropropionamide, 2010 grams of 40% trifluoroacetic acid aqueous solution and 5 grams of ferrous chloride into the three-necked flask, and stir The temperature was raised to 75°C, and the reaction was maintained for 20 hours. TLC detected that the reaction was complete, and fractional distillation was started to obtain 132 grams of the product with a GC content of 99.1% and a molar yield of 91%.

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PUM

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Abstract

The invention relates to a chemical synthesis process, and particularly relates to a process for synthesizing 2, 3, 3, 3-tetrafluoropropionic acid. According to the process, N, N-diethyl-2, 3, 3, 3-tetrafluoropropionamide as the starting material is subjected to a hydrolysis reaction under the acidic condition by using a catalyst; the side product N, N-diethyl-2, 3, 3, 3-tetrafluoropropionamide obtained by the fluorine substitution reaction of N, N-diethyl-1, 1, 2, 3, 3, 3-tetrafluoropropionamide is effectively utilized to obtain high-purity 2, 3, 3, 3-tetrafluoropropionic acid through the simple, easily-operated and easy separation and extraction process, the addition of the catalyst greatly accelerates the reaction speed and improves the product yield which reaches 96 percent, the benefit is built, the waste liquid treatment cost is reduced, and the environment is protected; the raw materials in the invention are low in price and easily obtained, the reaction conditions are mild, the reaction is speedy, the process is simple, easily operated and easily treated; and the process is beneficial for achievement of industrialization.

Description

[0001] technical field [0002] The invention relates to a chemical synthesis method, in particular to a synthesis method of 2,3,3,3-tetrafluoropropionic acid. Background technique [0003] 2,3,3,3-Tetrafluoropropionic acid is a valuable pharmaceutical and pesticide intermediate, CAS number: 359-49-9, and its molecular structure is as follows: [0004] [0005] At present, the main synthesis route of 2,3,3,3-tetrafluoropropionic acid is fluorine substitution by propionic acid. The disadvantage of this process is that the reaction is difficult to control, the by-products are many impurities, and it is not easy to purify, so the yield is not high. [0006] N,N-diethyl-2,3,3,3-tetrafluoropropionamide is N,N-diethyl-1,1,2,3,3,3-hexafluoropropylamine after fluorine substitution reaction The by-products are difficult to degrade, which greatly increases the difficulty and cost of factory waste liquid treatment, and if it is not handled properly, it will cause great pollution to...

Claims

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Application Information

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IPC IPC(8): C07C51/06C07C53/21
Inventor 张治国张伟略陈帅王久验
Owner 京山瑞生制药有限公司
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