Synthetic method for 4,4',6,6'-tetranitro-2,2'-diphenic acid

A technology of biphenyl dicarboxylic acid and tetranitro, which is applied in 4 fields, can solve the problems of small quantity and non-single product, and achieve the effect of low cost and simple method

Inactive Publication Date: 2014-02-19
INNER MONGOLIA UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the reported yield in this document is only 75%. At the same time, the number of nitro groups synthesized in the document is small and the product is not single. His synthetic route is to use concentrated nitric acid as a nitrating agent and react at 120 ° C for 5 hours to obtain dinitrobiphenyl A mixture of dicarboxylic acids

Method used

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  • Synthetic method for 4,4',6,6'-tetranitro-2,2'-diphenic acid
  • Synthetic method for 4,4',6,6'-tetranitro-2,2'-diphenic acid
  • Synthetic method for 4,4',6,6'-tetranitro-2,2'-diphenic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0027] 1. Add 11.28 g of 2,2'-biphenyldicarboxylic acid (prepared by yourself according to the method disclosed in the Journal of Dalian Institute of Technology, 1988, Volume 27 Supplement: 73-78) in a 500 mL three-necked flask. Under the condition of 15°C, stir continuously and slowly add 75mL of concentrated sulfuric acid (Sinopharm Chemical Reagent Co., Ltd., product number: 73108460), the color of the solution gradually turns orange during the acid addition process, and add all concentrated sulfuric acid After (approximately 2 hours), continue to stir for 10min;

[0028] 2. Measure 25mL of fuming nitric acid (Sinopharm Chemical Reagent Co., Ltd., article number: 10014617) and slowly add it dropwise to the above mixture. After dripping (approximately 1.5 hours), there was a small amount of brown gas in the bottle. Continue to stir for 30 minutes under ice bath conditions, then slowly raise the temperature to 90°C (heating time is 70 minutes), and keep it for 5 hours;

[00...

Embodiment 2

[0034] 1. Add 4.5g of 2,2'biphenyl dicarboxylic acid to a 250mL three-neck flask, and stir continuously under ice bath conditions and slowly add 30mL of concentrated sulfuric acid. After all the concentrated sulfuric acid is dropped, stir for 10min;

[0035] 2. Measure 10mL of fuming nitric acid and slowly add it to the above mixture. After the fuming nitric acid is dripped, stir for 30 minutes in an ice bath, then raise the temperature to 70°C and keep it for 5 hours;

[0036] 3. After the reaction is completed, cool down to room temperature, slowly add the mixture into a beaker with crushed ice, stir, and let stand;

[0037] 4. Suction filter the above mixture, wash with water three times, and dry to obtain 6.08 g of 4,4',6,6'-tetranitro-2,2'-biphenyldicarboxylic acid product.

[0038] The yield was calculated according to the method in Example 1, and the yield was 86%.

Embodiment 3

[0040] 1. Add 4.5g of 2,2′-biphenyldicarboxylic acid to a 250mL three-neck flask, and under ice bath conditions, continuously stir and slowly add 30mL of concentrated sulfuric acid, after all the concentrated sulfuric acid is dropped, stir for 10min;

[0041] 2. Measure 30mL of concentrated nitric acid and slowly add it to the above mixture. After the fuming nitric acid is dripped, stir for 30min in an ice bath, then raise the temperature to 90°C and keep it for 1h;

[0042] 3. After the reaction is completed, cool down to room temperature, slowly add the mixture into a beaker with crushed ice, stir, and let stand;

[0043] 4. Suction filter the above mixture, wash with water three times, and dry to obtain 5.77 g of 4,4',6,6'-tetranitro-2,2'-biphenyldicarboxylic acid product.

[0044] The yield was calculated according to the method in Example 1, and the yield was 85%.

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Abstract

The invention relates to a method for preparing 4,4',6,6'-tetranitro-2,2'-diphenic acid. According to the method, 2,2'-diphenic acid is used as a raw material directly; and 4,4',6,6'-tetranitro-2,2'-diphenic acid is obtained by a mixed acid nitration method. The method is simple in process and high in yield, and is suitable for production.

Description

technical field [0001] The invention relates to a preparation method of polynitro-substituted aromatic carboxylic acid, in particular to a synthesis method of 4,4',6,6'-tetranitro-2,2'-biphenyldicarboxylic acid. Background technique [0002] Polynitrobiphenyl carboxylic acid compounds are intermediates of various drugs, and can also be used as raw materials for pesticides, explosives and rubber vulcanization accelerators, especially in energetic materials. There are literature reports on the nitration reaction of 2,2'-biphenyl dicarboxylic acid, among which Yao Mengzheng and Li Yuesheng reported the research on the nitration and reduction reaction of 2,2'-biphenyl dicarboxylic acid (Journal of Dalian Institute of Technology, 1988, No. 27 Volume Suppl: 73-78). However, the reported yield in this document is only 75%. At the same time, the number of nitro groups synthesized in the document is small and the product is not single. His synthetic route is to use concentrated nitr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/57C07C201/08
Inventor 吴瑞凤施和平朱勇吉
Owner INNER MONGOLIA UNIV OF TECH
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