Preparation method of methyl difluoroacetate

A technology of methyl difluoroacetate and methyl dichloroacetate, applied in the field of preparation of methyl difluoroacetate, can solve problems such as unsuitable production, complexity, inconsistent catalyst selection and the like

Inactive Publication Date: 2012-07-04
SHANGHAI SINOFLUORO SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, some methods have synthetic steps that either use expensive reagents, making them complex and uneconomical for production, and there are inconsistencies in the choice of catalysts in the reaction routes.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] 33.6g methyl dichloroacetate was mixed with 9g potassium fluoride, reacted at 250 degrees centigrade for 6 hours, TLC showed that the raw material point was 1 hour (developing agent was glycerol: water=5: 1, the Rf=0.42 of the raw material=0.42. The Rf=0.81 of the product ), slowly added 80 ml of glycerin within 2 hours, cooled the system to below 0°C and kept it warm for 1 hour, stirred, distilled under reduced pressure, filtered, the precipitate was washed with toluene, and the filtrate was continued to be dried with anhydrous sodium sulfate. After the filter cake was driven off, 21.8 g of the product methyl difluoroacetate was obtained, with a yield of 82%.

Embodiment 2

[0012] 15.8g methyl dichloroacetate was mixed with 5g potassium fluoride, reacted at 200 degrees centigrade for 5 hours, TLC showed that the raw material point was 1 hour (developing agent was glycerol: water=5: 1, Rf=0.42 of raw material. Rf=0.81 of product ), slowly add 30 ml of glycerin within 1 hour, cool the system to below 0°C and keep it warm for 1 hour, stir, distill under reduced pressure, filter, wash the precipitate with toluene, and continue to dry the filtrate with anhydrous sodium sulfate. After the filter cake was driven off, 7.8 g of the product methyl difluoroacetate was obtained, with a yield of 68%.

Embodiment 3

[0014] Mix 80g of methyl dichloroacetate with 10g of potassium fluoride, react at 300 degrees Celsius for 6 hours, TLC shows that the raw material point is 1 hour (the developer is glycerol: water=5:1, the Rf of the raw material=0.42, the Rf of the product=0.81) 100 ml of glycerin was slowly added within 3 hours, the system was cooled to below 0°C and kept for 1 hour, stirred, distilled under reduced pressure, filtered, the precipitate was washed with toluene, and the filtrate was dried with anhydrous sodium sulfate. After the filter cake was driven off, 50.8 g of the product methyl difluoroacetate was obtained, with a yield of 80%.

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PUM

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Abstract

The invention relates to a method for preparing difluoromethyl acetate. The method is characterized by comprising the following steps of: mixing methyl dichloroacetate with potassium fluoride serving as a catalyst; reacting at a high temperature; slowly adding an organic solvent; cooling a system to be below zero DEG C and preserving heat; stirring; distilling under reduced pressure; filtering; washing a precipitate with methylbenzene; continually drying a filtrate with anhydrous sodium sulfate; and driving a filter cake away to obtain difluoromethyl acetate serving as a product.

Description

technical field [0001] The invention relates to the field of fluorine chemical industry, in particular to a preparation method of methyl difluoroacetate. Background technique [0002] Methyl difluoroacetate is a reagent used in organic synthesis, especially in the fields of agrochemistry and pharmacy. The proposed synthetic route to methyl difluoroacetate is not very economical. For example, some methods have synthetic steps that use expensive reagents, making them complex and uneconomical for production, and there are inconsistencies in the choice of catalysts in the reaction routes. Contents of the invention [0003] It is an object of the present invention to provide a process for the preparation of methyl difluoroacetate starting from readily available reagents. A process for the preparation of methyl difluoroacetate has now been found, characterized in that the process comprises the fluorination of methyl dichloroacetate in the presence of an effective amount of a c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/63C07C67/307B01J27/12
Inventor 闾肖波柳叶
Owner SHANGHAI SINOFLUORO SCI
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