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Preparation method of 4-bromo-3-fluorobenzoic acid

A technology of fluorobenzoic acid and potassium permanganate, which is applied in the field of preparation of 4-bromo-3-fluorobenzoic acid, can solve the problems of high yield and immiscibility of 4-bromo-3-fluorotoluene and potassium permanganate solution , It is difficult to produce chemical reactions and other problems, and achieve the effect of high yield and simplified operation process

Inactive Publication Date: 2017-11-07
BENGBU COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a kind of preparation method of 4-bromo-3-fluorobenzoic acid, this method solves the problem of 4-bromo-3-fluorotoluene and high manganese Potassium acid solution is immiscible and difficult to produce chemical reactions, the operation process is simplified, and the yield is higher

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] A preparation method of 4-bromo-3-fluorobenzoic acid, comprising the following steps:

[0017] (1) Oxidation: Add 100kg of 4-bromo-3-fluorotoluene, 120kg of water, and 0.1kg of Fatty alcohol polyether sodium sulfate (AES), heated to boiling reflux, then slowly add 167kg potassium permanganate under stirring condition, keep in boiling state, after reacting for 9 hours, stop the reaction after the reflux liquid no longer appears oil droplets;

[0018] (2) Filtration: Filtrate the reaction solution obtained in step (1) while hot to obtain a filtrate containing the target product 4-bromo-3-fluorobenzoic acid;

[0019] (3) Removal of potassium permanganate: In order to remove the remaining potassium permanganate in the filtrate, 0.1 kg of sodium sulfite should be added to the filtrate obtained in step (2). standard;

[0020] (4) Acidification: Slowly add concentrated hydrochloric acid with a concentration of 12mol / L to the solution obtained in step (3) under stirring. When...

Embodiment 2

[0025] A preparation method of 4-bromo-3-fluorobenzoic acid, comprising the following steps:

[0026] (1) Oxidation: Add 100kg of 4-bromo-3-fluorotoluene, 145kg of water, and 0.15kg of Fatty alcohol polyether sodium sulfate (AES), heated to boiling reflux, then slowly add 168kg parts of potassium permanganate under stirring condition, keep in boiling state, after reacting for 8 hours, stop the reaction after no more oil droplets appear in the reflux liquid ;

[0027] (2) Filtration: Filtrate the reaction solution obtained in step (1) while hot to obtain a filtrate containing the target product 4-bromo-3-fluorobenzoic acid;

[0028] (3) Removal of potassium permanganate: In order to remove residual potassium permanganate in the filtrate, 0.2 kg of sodium sulfite needs to be added to the filtrate obtained in step (2). The add-on of sodium sulfite takes the liquid that the purple color of the solution recedes and becomes transparent as the standard;

[0029] (4) Acidification:...

Embodiment 3

[0034] A preparation method of 4-bromo-3-fluorobenzoic acid, comprising the following steps:

[0035] (1) Oxidation: Add 100kg of 4-bromo-3-fluorotoluene, 150kg of water, and 0.2kg of Fatty alcohol polyether sodium sulfate (AES), heated to boiling reflux, then slowly add 169kg potassium permanganate under stirring condition, keep in boiling state, after reacting for 7 hours, stop the reaction after no more oil droplets appear in the reflux liquid;

[0036] (2) Filtration: Filtrate the reaction solution obtained in step (1) while hot to obtain a filtrate containing the target product 4-bromo-3-fluorobenzoic acid;

[0037] (3) Removal of potassium permanganate: In order to remove residual potassium permanganate in the filtrate, 0.3 kg of sodium sulfite needs to be added to the filtrate obtained in step (2). The add-on of sodium sulfite takes the liquid that the purple color of the solution recedes and becomes transparent as the standard;

[0038] (4) Acidification: Slowly add ...

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Abstract

The invention provides a preparation method of 4-bromo-3-fluorobenzoic acid. The 4-bromo-3-fluorobenzoic acid is prepared from 4-bromo-3-fluorotoluene used as a raw material with potassium permanganate used as an oxidant and used AES as a surfactant in the heating reflux state, the preparation process comprises the steps of oxidation, filtration, acidification, crystallization, filtration, washing and drying. By use of the surfactant and the oxidation technology in the boiling point state, the problem that 4-bromo-3-fluorotoluene and a potassium permanganate solution do not react with each other due to immiscibility is solved, the operation process is simplified, and the yield is higher.

Description

technical field [0001] The invention relates to a preparation method of 4-bromo-3-fluorobenzoic acid. Background technique [0002] 4-Bromo-3-fluorobenzoic acid is an important chemical raw material that can be used to prepare a variety of drugs (such as the anticancer drug bezamide). [0003] After a comprehensive search, no disclosure or report about the preparation method of 4-bromo-3-fluorobenzoic acid has been found. Contents of the invention [0004] The object of the present invention is to provide a kind of preparation method of 4-bromo-3-fluorobenzoic acid, this method solves the problem of 4-bromo-3-fluorotoluene and high manganese Potassium acid potassium solution is immiscible and difficult to produce chemical reactions, the operation process is simplified, and the yield is higher. [0005] The object of the present invention is achieved by the following technical scheme, a kind of preparation method of 4-bromo-3-fluorobenzoic acid, comprises the following st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C63/70C07C51/02C07C51/16C07C51/42
CPCC07C51/02C07C51/16C07C51/42C07C63/70
Inventor 郑桂富赵建军郭春燕
Owner BENGBU COLLEGE
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