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Method for producing and manufacturing difluorobenzophenone

The technology of a difluorobenzophenone and its manufacturing method is applied in the field of preparation of fluorine-containing intermediates, which can solve the problems of high production cost, low product purity, and high impurity content of difluorobenzophenone, and achieve easy industrial production, The effect of low impurity content and high purity

Pending Publication Date: 2022-01-21
济源市恒顺新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] For the 2,4 existing above / -The production cost of difluorobenzophenone is high, the content of impurities is high, the difficulty of separation is high, and the product purity is low. environment friendly

Method used

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  • Method for producing and manufacturing difluorobenzophenone
  • Method for producing and manufacturing difluorobenzophenone
  • Method for producing and manufacturing difluorobenzophenone

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0019] A method for producing difluorobenzophenone, comprising the following preparation steps:

[0020] S1. Add 166g of o-fluorotoluene into the reaction bottle, heat to reflux, and pass dry chlorine gas under light conditions. After reacting for 2 hours, add triethylamine, a side reaction inhibitor, to continue the reaction. After the reaction is completed, 312g of chlorinated solution is obtained. The reaction process is as follows :

[0021]

[0022] React under light in this step, the reaction obtains the mixture of p-fluorobenzyl chloride, p-fluorodichlorobenzyl, p-fluorotrichlorobenzyl The mixture is rectified, and the mixture of p-fluorobenzyl chloride and p-fluorodichlorobenzyl obtained through rectification purification is chlorinated again.

[0023] S2. Add 312 g of the chlorinated solution obtained in step S1 into the reaction bottle, start stirring and heating, heat to 120°C, and add 1.0‰ ferric chloride aqueous solution to it dropwise. Distillation, obtain o...

Embodiment 2

[0028] A method for producing difluorobenzophenone, comprising the following preparation steps:

[0029] S1. Add 166 g of o-fluorotoluene in the reaction bottle, heat to reflux, feed dry chlorine gas under light conditions, add side reaction inhibitor triethylamine after reacting for 2 hours, continue the reaction, and the reaction is completed to obtain 312 g of chlorinated solution;

[0030] React under light in this step, the reaction obtains the mixture of p-fluorobenzyl chloride, p-fluorodichlorobenzyl, p-fluorotrichlorobenzyl The mixture is rectified, and the mixture of p-fluorobenzyl chloride and p-fluorodichlorobenzyl obtained through rectification purification is chlorinated again.

[0031] S2. Add 312 g of the chlorinated solution obtained in step S1 into the reaction bottle, start stirring and heating, heat to 120°C, and add 1.0‰ ferric chloride aqueous solution to it dropwise. Distillation, to obtain o-fluorobenzoyl chloride 210g;

[0032] S3. Add 215g of fluorob...

Embodiment 3

[0034] A method for producing difluorobenzophenone, comprising the following preparation steps:

[0035] S1. Add 166 g of o-fluorotoluene in the reaction bottle, heat to reflux, feed dry chlorine gas under light conditions, add side reaction inhibitor triethylamine after reacting for 2 hours, continue the reaction, and the reaction is completed to obtain 312 g of chlorinated solution;

[0036] React under light in this step, the reaction obtains the mixture of p-fluorobenzyl chloride, p-fluorodichlorobenzyl, p-fluorotrichlorobenzyl The mixture is rectified, and the mixture of p-fluorobenzyl chloride and p-fluorodichlorobenzyl obtained through rectification purification is chlorinated again.

[0037] S2. Add 312 g of the chlorinated solution obtained in step S1 into the reaction bottle, start stirring and heating, heat to 120°C, and add 1.0‰ ferric chloride aqueous solution to it dropwise. Distillation, to obtain o-fluorobenzoyl chloride 210g;

[0038] S3. Add 215g of fluorob...

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Abstract

The invention belongs to the technical field of chemical synthesis, and particularly relates to a method for producing and manufacturing difluorobenzophenone. O-fluorotoluene used as a raw material is mixed with fluorobenzene after being subjected to photochlorination and catalytic hydrolysis, high-purity 2, 4 / -difluorobenzophenone is obtained under the catalysis of a mixed catalyst of anhydrous aluminum chloride and lithium chloride, the used raw material is cheap and easy to obtain, the synthesis route is simple, operation is easy, and industrial production is facilitated. Fluorobenzene is used as a solvent and can be recycled; and washing water is circularly used for quenching reaction, an aluminum trichloride solution generated by a quenching reaction can be used for producing a water purifying agent, no wastewater is generated in the whole reaction process, the environment-friendly effect is achieved, and resources are saved.

Description

technical field [0001] The invention relates to the technical field of preparation of fluorine-containing intermediates, in particular to a production method of difluorobenzophenone. Background technique [0002] 2,4 / - Difluorobenzophenone is an oily liquid with a relative density of 1.244. It is insoluble in water and soluble in organic solvents such as benzene, xylene, and ketone. It is an intermediate of the fungicide triconazole, which was produced by Zenecaol in the United Kingdom in 1980. The company has successfully developed a sterol demethylation inhibitor, which can effectively inhibit the biosynthesis of ergosterol, can cause fungal cell wall rupture, and has good protective and therapeutic effects on many diseases caused by basidiomycetes and ascomycetes. fumigation effect, but inactive to oomycetes and bacteria. [0003] 2,4 / - Difluorobenzophenone, as an important intermediate for the synthesis of tributazone, due to high production costs, many by-product...

Claims

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Application Information

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IPC IPC(8): C07C45/41C07C49/813
CPCC07C17/14C07C51/58C07C45/41C07C25/13C07C63/68C07C49/813
Inventor 马立强张伟任建军
Owner 济源市恒顺新材料有限公司