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Preparation method of 3,5-difluoroanisole

A technology of difluoroanisole and trifluorobenzene, which is applied in the field of preparation of organic compounds, can solve the problems of long reaction time, low yield, and only 68% yield, and achieve the effect of high product yield and high purity

Active Publication Date: 2009-04-15
HEBEI MAIERSTON ELECTRONICS MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] Raw materials 3,5-difluoroaniline and 3,5-dinitrophenol are relatively expensive, so the cost of the synthesized chronoform 3,5-difluoroanisole is relatively high, so it is not suitable to use the first two synthetic routes
The raw material 2,4-difluoroaniline used in the third and fourth process routes is easy to get, and the process is feasible, but the reaction time is longer and the yield is lower
The fifth process is feasible, but the reaction time is longer and the yield is lower
Although the sixth route has mild reaction conditions, the raw material yield is high and the yield is only 68%.

Method used

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  • Preparation method of 3,5-difluoroanisole
  • Preparation method of 3,5-difluoroanisole
  • Preparation method of 3,5-difluoroanisole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] In a 5L three-necked flask equipped with a thermometer, a spherical condenser and a mechanical stirrer, add a solution containing 10.72mol (578.8g) of sodium methoxide at room temperature, the concentration of the sodium methoxide solution is 20% in terms of methanol, and then 938mL of solvent Methanol was slowly added into the three-necked flask, and stirred evenly at a slow speed.

[0056] Under the condition of stirring, 5.36mol (708g) of 1,3,5-trifluorobenzene was added dropwise into the reaction flask, and heated to raise the temperature, so that the reaction was carried out at 70-80°C. After the reaction was carried out for 5 hours, Heating was stopped, and the reaction product was allowed to cool naturally.

[0057] The cooled reaction product is carried out aftertreatment, and described aftertreatment comprises

[0058] 1) The reaction product is subjected to suction filtration to obtain a solid and a filtrate, and the solid is washed twice with methanol; after...

Embodiment 2

[0063] In a 5L three-necked flask equipped with a thermometer, a spherical condenser and a mechanical stirrer, add a solution containing 5.36mol (289.44g) of sodium methoxide at room temperature. The concentration of the sodium methoxide solution is 30% in terms of methanol, and then 1000mL of solvent Slowly add toluene into the three-necked flask, and stir evenly at a slow speed.

[0064] Under the condition of stirring, 5.36mol (708g) of 1,3,5-trifluorobenzene was added dropwise into the reaction flask, and heated to raise the temperature, so that the reaction was carried out at 60-80°C. After the reaction was carried out for 10 hours, Heating was stopped, and the reaction product was allowed to cool naturally.

[0065] The cooled reaction product is carried out aftertreatment, and described aftertreatment comprises

[0066] 1) The reaction product is subjected to suction filtration to obtain a solid and a filtrate, and the solid is washed twice with methanol; after the fil...

Embodiment 3

[0071] In a 5L three-neck flask equipped with a thermometer, a spherical condenser and a mechanical stirrer, add a solution containing 8.04mol (434.16g) of sodium methoxide at room temperature. The concentration of the sodium methoxide solution is 40% in terms of methanol, and then 950mL of solvent Dimethylformamide was slowly added into the three-necked flask, and stirred evenly at a slow speed.

[0072] Under the condition of stirring, 5.36mol (708g) of 1,3,5-trifluorobenzene was added dropwise into the reaction flask, and heated to raise the temperature, so that the reaction was carried out at 60-100°C. After the reaction was carried out for 18 hours, Heating was stopped, and the reaction product was allowed to cool naturally.

[0073] The cooled reaction product is carried out aftertreatment, and described aftertreatment comprises

[0074] 1) The reaction product is subjected to suction filtration to obtain a solid and a filtrate, and the solid is washed twice with methan...

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Abstract

The invention relates to preparation of an organic compound, particularly to a method for preparing 3, 5-difluoro anisole, which belongs to the field of organic compound preparation technology. With the preparation of the organic compound, reaction products are obtained through a reaction between 1, 3, 5-trifluoro-benzene and sodium methoxide solution with the presence of solvent; then a post treatment is carried out to the reaction products to get 3, 5-difluoro anisole; the prepared product 3, 5-difluoro anisole has high purity and high product yield coefficient; in addition, the reaction steps are few and the production cycle of the product is short.

Description

technical field [0001] The invention relates to the preparation of an organic compound, in particular to a method for preparing 3,5-difluoroanisole, which belongs to the technical field of organic compound preparation. Background technique [0002] 3,5-Difluoroanisole is an important fine organic synthesis intermediate, mainly used in the synthesis of pesticides, medicines and liquid crystal materials. [0003] For the preparation method of 3,5-difluoroanisole, there have been many researches at home and abroad. The "3,5-difluoroanisole The preparation method " discloses several methods for preparing 3,5-difluoroanisole in the prior art: [0004] (1) Using 3,5-difluoroaniline as a raw material, it is prepared by diazotization, bromination, and methoxylation; [0005] (2) Using 3,5-dinitrophenol as a raw material, it is prepared by high-temperature fluorination and methoxylation; [0006] (3) Using 2,4-difluoroaniline as raw material, it can be prepared by bromination, dia...

Claims

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Application Information

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IPC IPC(8): C07C43/225C07C41/01
Inventor 仲锡军刘江宏于志广
Owner HEBEI MAIERSTON ELECTRONICS MATERIAL
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