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Method for preparing 3-chlorine-5-bromophenol

A technology of bromophenol and nitroaniline, which is applied in the field of preparation of 3-chloro-5-bromophenol, can solve the problems such as the preparation method of 3-chloro-5-bromophenol has not been retrieved, and achieves simple and easy to operate post-processing, The effect of high reaction yield and mild reaction conditions

Active Publication Date: 2011-08-10
中国中化股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the preparation method of 3-chloro-5-bromophenol has not been retrieved

Method used

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  • Method for preparing 3-chlorine-5-bromophenol
  • Method for preparing 3-chlorine-5-bromophenol
  • Method for preparing 3-chlorine-5-bromophenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 1) Bromine substitution reaction:

[0036] Add 69 parts of 2-chloro-4-nitroaniline and 210 parts of glacial acetic acid into the reaction kettle and stir, add 70 parts of liquid bromine dropwise at room temperature, and continue stirring for 2 hours after adding, pour the reaction mixture into another In the reactor of 1000 parts of ice water, a large number of yellow solids were precipitated. The yellow solid was filtered, washed thoroughly with ice water, and dried at room temperature to obtain 90 parts of yellow-green solid product 2-chloro-4-nitro-6-bromoaniline.

[0037] 2) Hydrogen substitution reaction after diazotization:

[0038] Add the above 90 parts of 2-chloro-4-nitro-6-bromoaniline, 110 parts of concentrated sulfuric acid, and 450 parts of ethanol into the reaction kettle, heat up to 70°C under stirring and react for 30 minutes, and then batch to Add 55 parts of sodium nitrite into the reaction kettle, continue to stir at 70°C for 3 hours after the addit...

Embodiment 2

[0045]The steps 1), 2) and 3) were carried out in the same manner as in Example 1 to obtain the diazonium salt solution in 4). Add 70 parts of water and 140 parts of concentrated sulfuric acid into another reaction kettle, then heat up to 80°C, and add the prepared diazonium salt solution dropwise while stirring, stir for 2.5 hours after the dropwise addition, and let it stand to cool to room temperature , extracted twice with methyl tert-butyl ether, then the organic phase was washed with water and then with 20% aqueous sodium hydroxide. Combine the lye and adjust the pH value to 3-4 with concentrated hydrochloric acid. Fully extracted with methyl tert-butyl ether, the organic extract layer was washed with water, dried over anhydrous sodium sulfate, filtered to remove the desiccant, and then precipitated to obtain 25 parts of solid product 3-chloro-5-bromophenol.

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Abstract

The invention relates to a method for preparing 3-chlorine-5-bromophenol. In the method, 2-chlorine-4-nitroaniline is used as the raw material; and the 3-chlorine-5-bromophenol is prepared according to the following process. In the preparation method, the raw material has low price and is easily obtained; the reaction steps are simple; the reaction condition is mild; the reaction yield is high; the post treatment is simple and is easy to operate; and the product has high content.

Description

technical field [0001] The invention relates to the field of medicine, in particular to a preparation method of 3-chloro-5-bromophenol. Background technique [0002] 3-Chloro-5-bromophenol is an important pharmaceutical intermediate, which can be used in the preparation of various pharmaceutical products. At present, the preparation method of 3-chloro-5-bromophenol has not been retrieved yet. Contents of the invention [0003] The purpose of this invention is to provide a kind of preparation method of 3-chloro-5-bromophenol. [0004] In order to realize the purpose of the present invention, the present invention provides a kind of preparation method of 3-chloro-5-bromophenol, and this method comprises the following steps: [0005] 1) take 2-chloro-4-nitroaniline as raw material, form the compound represented by formula I by bromination reaction according to the following route: [0006] [0007] 2) make the compound represented by formula I form the compound represen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/27C07C37/045
Inventor 郭湘云陆慧李新平叶挺勋
Owner 中国中化股份有限公司
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