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2,3,3,3-tetrafluoro propionic acid (i) synthesis method

A technique for the synthesis of tetrafluoropropionic acid, applied in organic chemistry, amide preparation, etc., can solve the problems of high cost of harmless treatment, environmental impact, etc., and achieve the effects of low production cost, mild reaction conditions, and easy operation

Inactive Publication Date: 2014-01-15
赵磊 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Benefits of technology

In this new process described in this patented technology, two different chemical compounds are combined at an intermediate stage during which they react together without generating unwanted side products such as chlorofluoroformate esters that can be harmful when used on food items like milk. By combining these chemically active molecules into one substance instead of creating them separately from other materials, it becomes easier to produce consistency between each batch produced while reducing costs compared to traditional methods.

Problems solved by technology

This patents discusses methods for producing various compounds from halogen tripodazole or tetrahydrofuran without generating excessive amounts of wastes during their manufacture processes. Existing techniques involve complicated operations involving multiple materials like metal salt precursors, solvent extraction/liquid phase separation, purification, etc., leading to increased operating expenses and potential negative effects on both consumable resources and natural environments.

Method used

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Examples

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Effect test

example 1

[0044] Example 1: Preparation of 2,3,3,3-tetrafluoropropionic acid (I).

[0045]Put N,N-diethyl-2,3,3,3-tetrafluoropropionamide (II) (300g, 1.49mol), 37% hydrochloric acid (700ml), ethanol (1000ml), water (100ml) into the reaction In the bottle, heat up and reflux for 10 hours. After the reaction is complete, distill at atmospheric pressure and collect 120°C fractions to obtain 207g of I, with a yield of 95% and a purity of 98.5% (detected by gas chromatography);

[0046] The preparation conditions are:

[0047] N, N-dialkyl-2,3,3,3-tetrafluoropropionamide (II) is hydrolyzed under the action of hydrochloric acid.

[0048] The hydrolysis reaction uses a mixed solvent of ethanol and water with a volume ratio of 10:1.

[0049] The reaction temperature is controlled at 90-120°C.

[0050] The reaction time is controlled at 10-24 hours.

[0051] The molar ratio of N,N-dialkyl-2,3,3,3-tetrafluoropropionamide (II) to acid or base is 1:5-10.

[0052] The weight to volume ratio of ...

example 2

[0053] Example 2: Preparation of 2,3,3,3-tetrafluoropropionic acid (I).

[0054] Put N,N-diethyl-2,3,3,3-tetrafluoropropionamide (300g, 1.49mol), 98% sulfuric acid (600ml), ethanol (1000ml), water (100ml) into the reaction flask, Heated and refluxed for 12 hours, the reaction was completed, distilled at atmospheric pressure, and collected 120 ° C fractions to obtain 200 g of I, with a yield of 92% and a purity of 98.3% (detected by gas chromatography);

[0055] The preparation conditions are:

[0056] N, N-dialkyl-2,3,3,3-tetrafluoropropionamide (II) is hydrolyzed under the action of hydrochloric acid.

[0057] The hydrolysis reaction uses a mixed solvent of ethanol and water with a volume ratio of 10:1.

[0058] The reaction temperature is controlled at 90-120°C.

[0059] The reaction time is controlled at 10-24 hours.

[0060] The molar ratio of N,N-dialkyl-2,3,3,3-tetrafluoropropionamide (II) to acid or base is 1:5-10.

[0061] The weight to volume ratio of N,N-dialkyl...

example 3

[0062] Example 3: Preparation of 2,3,3,3-tetrafluoropropionic acid (I)

[0063] N, N-diethyl-2,3,3,3-tetrafluoropropionamide (II) (300g, 1.49mol), 98% sulfuric acid (600ml), ethanol (1000ml), water (100ml), dihydrate Cupric chloride (2.54g, 0.0149mol) was placed in a reaction flask, heated and refluxed for 5 hours, after the reaction was completed, distilled at atmospheric pressure, and 208g of I was obtained by collecting fractions at 120°C, with a yield of 96% and a purity of 99.0% (detected by gas chromatography) ;

[0064] The preparation conditions are:

[0065] N, N-dialkyl-2,3,3,3-tetrafluoropropionamide (II) is hydrolyzed under the action of hydrochloric acid.

[0066] The hydrolysis reaction uses a mixed solvent of ethanol and water with a volume ratio of 10:1.

[0067] The reaction temperature is controlled at 90-120°C.

[0068] The reaction time is controlled at 10-24 hours.

[0069] The molar ratio of N,N-dialkyl-2,3,3,3-tetrafluoropropionamide (II) to acid or...

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Abstract

The present invention belongs to the technical field of organic chemistry, and provides a 2,3,3,3-tetrafluoro propionic acid (I) synthesis method, which comprises that: under an acid or base condition, in the presence of a catalyst or without a catalyst system, N,N-dialkyl-2,3,3,3-tetrafluoropropionamide (II) is subjected to hydrolysis to obtain 2,3,3,3-tetrafluoro propionic acid (I). The synthesis method has characteristics of simple operation, low production cost, high product purity, mild reaction condition, and the like, and is suitable for industrial production.

Description

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Claims

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Application Information

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Owner 赵磊
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