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

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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