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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: 2020-04-21
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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  • Preparation method of 3, 3, 3-trifluoropropionic acid
  • Preparation method of 3, 3, 3-trifluoropropionic acid
  • 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 reaction kettle, vacuumize, draw in 1000mL anhydrous tetrahydrofuran, Feed 250g (2.54mol) of 2-chloro-1-1-difluoroethylene under stirring, raise the temperature to 80°C, feed carbon monoxide to a pressure of 0.8 MPa, keep warm until the pressure no longer drops, and then continue to feed carbon monoxide to a pressure of 0.8 MPa , pass through three times, pass through time 5 hours, stop reaction. Cool down to room temperature, filter and recover divalent palladium and nickel powder, quickly distill the filtrate under normal pressure to obtain a mixed solution of organic solvent and product, then rectify and recover the organic solvent, collect the fraction at 70-72°C, which is 3,3-difluoro- 2-acryloyl chloride weighs 263.8g, and the yield is 82.15%.

[0038] (2) Vacuumize the 2L M...

Embodiment 2

[0041] This embodiment includes the following steps:

[0042](1): Add 6.3g of palladium acetate (28.1mmol), 1.7g of nickel powder (29.0mmol) and 14.6g of triphenylphosphine (55.6mmol) into a 2L stainless steel reaction kettle, vacuumize, and suck in 1000mL of anhydrous tetrahydrofuran, Feed 275g (2.79mol) of 2-chloro-1-1-difluoroethylene under stirring, raise the temperature to 90°C, feed carbon monoxide to a pressure of 0.8 MPa, keep warm until the pressure no longer drops, and then continue to feed carbon monoxide to a pressure of 0.8 MPa , pass through three times, pass through time 5 hours, stop reaction. Cool down to room temperature, filter and recover divalent palladium and nickel powder, quickly distill the filtrate under normal pressure to obtain a mixed solution of organic solvent and product, then rectify and recover the organic solvent, collect fractions at 70-72°C to obtain 3,3-difluoro-2- Acryloyl chloride weighs 281.9g, and the yield is 79.8%.

[0043] (2): Va...

Embodiment 3

[0046] This embodiment includes the following steps:

[0047] (1) Add 2.5g (14.1mmol) palladium chloride, 1.7g (29.0mmol) nickel powder and 15.3g (58.3mmol) triphenylphosphine in 2L stainless steel reactor, vacuumize, suck in 1240mL anhydrous tetrahydrofuran, Feed 275g (2.79mol) of 2-chloro-1-1-difluoroethylene under stirring, raise the temperature to 80°C, feed carbon monoxide to a pressure of 0.8 MPa, keep warm until the pressure no longer drops, then continue to feed carbon monoxide to a pressure of 0.8 MPa , pass through three times, pass through time 6 hours, stop reaction. Cool down to room temperature, filter and recover divalent palladium and nickel powder, quickly distill the filtrate under normal pressure to obtain a mixed solution of organic solvent and product, then rectify and recover the organic solvent, collect the fraction at 70-72°C, which is 3,3-difluoro 2 - acryloyl chloride, heavy 278g, yield 78.7%.

[0048] (2) Vacuumize the 2L Monel reactor, pump in 278...

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Abstract

The invention discloses a preparation method of 3, 3, 3-trifluoropropionic acid. The preparation method comprises the following steps: firstly, taking 2-chloro-1-1-difluoroethylene (a) as a raw material and carrying out a carbonylation reaction between the raw material and carbon monoxide to obtain 3, 3-difluoro-2-allyl chloride (b); carrying out a fluorination reaction on 3, 3-difluoro 2-allyl chloride by using hydrogen fluoride (HF) to obtain 3, 3, 3-trifluoropropionyl fluoride (c); and finally hydrolyzing the 3, 3, 3-trifluoropropionyl fluoride to obtain trifluoropropionic acid (d). The preparation method has the advantages as follows: the raw materials are cheap and easily available; conditions are mild; conversion rate of the starting material is high; and the total yield of the three-step reactions can reach 50% or above.

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 The special group can effectively enhance the polarity, stability and lipophilicity of the substance, and has unique excellent properties. It is an important intermediate for the synthesis of many fluorine-containing medicines, pesticides and polymer materials, and has a wide range of applications. [0003] 3,3,3-Trifluoropropionic acid is a colorless, toxic and highly corrosive liquid, which can be miscible with water and various organic solvents...

Claims

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Application Information

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Patent Type & Authority Applications(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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