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A kind of preparation method of 3,3,3-trifluoropropionic acid

A technology of trifluoropropionic acid and trifluoropropionyl, which is applied in the field of preparation of 3,3,3-trifluoropropionic acid, can solve the problems of expensive raw materials and reagents, low yield and the like, and achieves improved conversion rate and selectivity, The effect of high conversion and mild reaction conditions

Active Publication Date: 2022-06-03
湖南有色郴州氟化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Although there are many preparation methods disclosed above, there are disadvantages such as low yield or expensive raw material reagents

Method used

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  • A kind of preparation method of 3,3,3-trifluoropropionic acid
  • A kind of preparation method of 3,3,3-trifluoropropionic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] This embodiment includes the following steps:

[0037] (1) add 4.5g (25.4mmol) palladium chloride, 1.5g (25.6mmol) nickel powder and 13.3g (50.8mmol) triphenylphosphine in 2L stainless steel reactor, vacuumize, suck in 1000mL anhydrous tetrahydrofuran, Under stirring, feed 250g (2.54mol) of 2-chloro-1-1-difluoroethylene, be warming up to 80°C, feed carbon monoxide to a pressure of 0.8MPa, and continue to feed carbon monoxide to a pressure of 0.8MPa after the insulation reaction until the pressure no longer decreases. , pass three times, pass time 5 hours, stop the reaction. Cool to room temperature, filter and recover divalent palladium and nickel powder, rapidly distill the filtrate at atmospheric pressure to obtain a mixed solution of organic solvent and product, then rectify and recover the organic solvent, and collect fractions at 70 to 72 °C, which is 3,3-difluoro- 2-Acryloyl chloride, weight 263.8 g, yield 82.15%.

[0038] (2) vacuumize the 2L Monel reaction ket...

Embodiment 2

[0041] This embodiment includes the following steps:

[0042](1): add 6.3g palladium acetate (28.1mmol), 1.7g nickel powder (29.0mmol) and 14.6g triphenylphosphine (55.6mmol) in 2L stainless steel reactor, vacuumize, suck in 1000mL anhydrous tetrahydrofuran, Under stirring, feed 275g (2.79mol) of 2-chloro-1-1-difluoroethylene, be warming up to 90°C, feed carbon monoxide to a pressure of 0.8MPa, and continue to feed carbon monoxide to a pressure of 0.8MPa after the insulation reaction until the pressure no longer decreases. , pass three times, pass time 5 hours, stop the reaction. Cool to room temperature, filter and recover divalent palladium and nickel powder, rapidly distill the filtrate at atmospheric pressure to obtain a mixed solution of organic solvent and product, then rectify and recover the organic solvent, and collect fractions at 70 to 72 °C to obtain 3,3-difluoro2- Acryloyl chloride, weight 281.9 g, yield 79.8%.

[0043] (2): evacuating the 2L Monel reactor, pump...

Embodiment 3

[0046] This embodiment includes the following steps:

[0047] (1) 2.5g (14.1mmol) of palladium chloride, 1.7g (29.0mmol) of nickel powder and 15.3g (58.3mmol) of triphenylphosphine were added to the 2L stainless steel reactor, evacuated, and 1240mL of anhydrous tetrahydrofuran was sucked in, Under stirring, feed 275g (2.79mol) of 2-chloro-1-1-difluoroethylene, be warming up to 80°C, feed carbon monoxide to a pressure of 0.8MPa, and continue to feed carbon monoxide to a pressure of 0.8MPa after the insulation reaction until the pressure no longer decreases. , pass three times, pass time 6 hours, stop the reaction. Cool down to room temperature, filter and recover divalent palladium and nickel powder, rapidly distill the filtrate at atmospheric pressure to obtain a mixed solution of organic solvent and product, then rectify and recover the organic solvent, and collect 70-72 °C fraction, which is 3,3-difluoro2 -Acryloyl chloride, weight 278g, yield 78.7%.

[0048] (2) vacuumize...

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Abstract

A preparation method of 3,3,3-trifluoropropionic acid. The preparation method of the present invention first uses 2-chloro-1-1-difluoroethylene (a) as a raw material to perform carbonyl insertion reaction with carbon monoxide to obtain 3,3-difluoro 2-acryloyl chloride (b); then use HF to treat 3 ,3‑Difluoro 2‑acryloyl chloride is subjected to fluorination reaction to obtain 3,3,3‑trifluoropropionyl fluoride (c), and finally 3,3,3‑trifluoropropionyl fluoride is hydrolyzed to obtain trifluoropropionyl fluoride Acid (d). The preparation method of the invention has cheap and easy-to-obtain raw materials, mild conditions, high conversion rate of starting materials, and the total yield of the three-step reaction can reach more than 50%.

Description

technical field [0001] The invention relates to the field of chemical intermediates, in particular to a preparation method of 3,3,3-trifluoropropionic acid. Background technique [0002] In recent years, fluorine-containing compounds have attracted the attention of researchers at home and abroad, and have been widely used in medicine, pesticides, materials, refrigerants and other fields. As an important organic chemical intermediate, 3,3,3-trifluoropropionic acid is mainly used in medicine and pesticides. Because it contains CF 3 Special groups can effectively enhance the polarity, stability and lipophilicity of substances, and have unique and excellent properties. They are important intermediates for the synthesis of many fluorine-containing pharmaceuticals, pesticides and polymeric materials, and have a wide range of applications. [0003] 3,3,3-Trifluoropropionic acid is a colorless, toxic and highly corrosive liquid, which is miscible with water and various organic sol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/04C07C53/18
CPCC07C51/58C07C51/62C07C51/04C07C55/40C07C53/48Y02P20/584
Inventor 王刚李志鹏彭智敏尹德美张振华
Owner 湖南有色郴州氟化学有限公司
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