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A method of co-producing 2-fluoropropionate and ethyl difluoroacetate

A technology of ethyl difluoroacetate and fluoropropionate, which is applied in the field of co-production of 2-fluoropropionate and ethyl difluoroacetate, and can solve the problems of low fluorination yield of potassium fluoride, large amount of solvent recovery, and three wastes and other problems, to achieve the effect of mild reaction conditions, simple process and low cost

Active Publication Date: 2022-06-21
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The preparation methods of above-mentioned various 2-fluoropropionates all have certain weak point: (1) take 2-methyl chloropropionate as raw material, though cost is low, use Potassium Fluoride fluorination yield low, produce The amount of "three wastes" is extremely large
The risk of fluorination with hydrogen fluoride is high, the equipment is severely corroded, and it is difficult to dispose of the spent catalyst; (2) the raw material process route is high with 2-bromopropionate; (3) the raw material is prepared with 2-hydroxypropionate The 2-fluoropropionate process route has a large amount of solvent recovery, and post-treatment brings a lot of "three wastes"

Method used

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  • A method of co-producing 2-fluoropropionate and ethyl difluoroacetate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036](1) Place tetrafluoroethyldimethylamine (TFEDMA) in a 500ml tetrafluoro-lined reactor with a condenser, slowly drip methyl lactate under 0°C, tetrafluoroethyldimethylamine and The molar ratio of methyl lactate is 1:1, the temperature of the control system is lower than 10 °C, the temperature is raised to 40 °C after the addition, stirred for 5 h, the reaction is completed, the temperature is lowered to 0 °C, and triethylamine, triethylamine and tetrafluoroethyl are slowly added. The molar ratio of dimethylamine is 0.25:1, and rectification under reduced pressure obtains methyl 2-fluoropropionate and N,N-dimethyldifluoroacetamide, and the yield of methyl 2-fluoropropionate is 98.92%. ;

[0037] (2) The N,N-dimethyldifluoroacetamide obtained in step (1) and absolute ethanol were placed in a 500ml four-necked round-bottomed flask, absolute ethanol and N,N-dimethyldifluoroacetamide were The molar ratio of the sulphuric acid is 1:1, and 98wt% of concentrated sulfuric acid is...

Embodiment 2

[0039] (1) Place tetrafluoroethyldimethylamine (TFEDMA) in a 500ml tetrafluoro-lined reactor with a condenser, slowly drip ethyl lactate under 0°C, tetrafluoroethyldimethylamine and The molar ratio of ethyl lactate was 1.2:1, the temperature of the control system was lower than 10 °C, the temperature was raised to 50 °C after the addition was completed, stirred for 4 h, the reaction was completed, the temperature was lowered to 0 °C, and 4-N,N-lutidine ( C 7 H 10 N 2 ), the molar ratio of 4-N,N-lutidine and tetrafluoroethyldimethylamine is 0.3:1, and rectification under reduced pressure obtains ethyl 2-fluoropropionate and N,N-dimethyldimethylamine Fluoroacetamide, the yield of ethyl 2-fluoropropionate was 96.62%;

[0040] (2) The N,N-dimethyldifluoroacetamide obtained in step (1) and absolute ethanol were placed in a 500ml four-necked round-bottomed flask, absolute ethanol and N,N-dimethyldifluoroacetamide were The molar ratio of the concentrated sulfuric acid is 1.3:1, a...

Embodiment 3

[0042] (1) Put tetrafluoroethyldimethylamine (TFEDMA) in a 500ml tetrafluoro-lined reaction kettle with a condenser, slowly drip trifluoropropyl lactate, tetrafluoroethyldimethylamine at 0°C The molar ratio of amine to trifluoropropyl lactate was 1.5:1, the temperature of the system was controlled to be lower than 10 °C, the temperature was raised to 60 °C after the addition was completed, stirred for 3 h, the reaction was completed, the temperature was lowered to 0 °C, and N-cyclohexyl-N- Cyclopentyl-N-ethylamine (C 13 H 25 N), the molar ratio of N-cyclohexyl-N-cyclopentyl-N-ethylamine and tetrafluoroethyldimethylamine is 0.35:1, and rectification under reduced pressure obtains trifluoropropyl 2-fluoropropionate and N,N-dimethyldifluoroacetamide, the yield of trifluoropropyl 2-fluoropropionate was 97.52%;

[0043] (2) The N,N-dimethyldifluoroacetamide obtained in step (1) and absolute ethanol were placed in a 500ml four-necked round-bottomed flask, absolute ethanol and N,N-...

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Abstract

The invention discloses a method for co-producing 2-fluoropropionate and ethyl difluoroacetate, comprising: (a) reacting a fluorinating reagent and lactate at a molar ratio of 0.5 to 2:1, and the reaction temperature is 30~120℃, the reaction time is 0.5~7h. After the reaction, the temperature of the reaction material is lowered, nitrogen-containing compounds are added, and the 2-fluoropropionate product and N,N-dimethyldifluoroacetamide are obtained by rectification under reduced pressure; (b) adding concentrated sulfuric acid to the mixture of absolute ethanol and N,N-dimethyl difluoroacetamide obtained in step (a) to react, the mixture of absolute alcohol and N,N-dimethyl difluoroacetamide The molar ratio is 0.5-4.5:1, the molar ratio of concentrated sulfuric acid to N,N-dimethyldifluoroacetamide is 0.1-1.5:1, the reaction temperature is 50-170°C, the reaction time is 1-10h, and the reaction is over Cooling, liquid separation, rectification to obtain ethyl difluoroacetate product. The invention has the advantages of environmental protection, high yield and low cost.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a method for co-producing 2-fluoropropionate and ethyl difluoroacetate. Background technique [0002] Fluorine-containing polymer materials have the advantages of high glass transition temperature, low surface energy, and anti-aging. In particular, the new fluorine-containing polymer optical fiber materials are much better than traditional optical fibers in the main performance indicators such as signal attenuation and heat resistance. At present, the main monomer for the preparation of fluorine-containing polymer materials is 2-fluoroacrylate, and 2-fluoropropionate is a key intermediate in the preparation of 2-fluoroacrylate. Ethyl difluoroacetate is a widely used chemical product, which can be used to prepare various fluorinated pesticides, pharmaceutical intermediates, etc., and has a large market scale. [0003] The synthetic method of 2-fluoropropionate mainly includes th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/48C07C67/307C07C69/63C07C67/20
CPCC07C67/20C07C67/307C07C67/48C07C69/63
Inventor 吕杨李宏峰叶立峰马利勇张万宏
Owner JUHUA GROUP TECH CENT