Synthetic method of 2,4,6-trichloro-3-nitrobenzoic acid

A technology of nitrobenzoic acid and synthesis method, which is applied in the field of compound synthesis, and can solve problems such as outdated technology, difficult management, and long process

Inactive Publication Date: 2016-07-20
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] 2,4,6-Trichloro-3-nitrobenzoic acid is an organic chemical intermediate, which is widely used in the synthesis of chromogens and has a wide range of uses. There are dozens of varieties of chromogens synthesized with it. Chromogen has unique functions, and is a promising chromogen and synthetic chromogen intermediate, but 2,4,6-trichloro-3-nitrobenzoic acid has never been ideal for industrial production method
The traditional production process of 2,4,6-trichloro-3-nitrobenzoic acid is backward, the process is long, the yield is low, the amount of three wastes is large, and it is difficult to treat

Method used

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  • Synthetic method of 2,4,6-trichloro-3-nitrobenzoic acid

Examples

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example 1

[0016] Add 10mL of m-aminobenzoic acid with a concentration of 0.1mol / L to a 250mL round bottom flask, then add 50mL of anhydrous ether, place it on a magnetic stirrer, and stir at a speed of 300r / min for 10min to fully dissolve it; keep the magnetic stirring speed While stirring, chlorine gas was introduced into the flask at a rate of 10mL / min, 10mL was ventilated, the shaking table was shaken for 30min, then 100mL of deionized water was added, stirring was continued for 10min, and the mixture was put into a Buchner funnel for extraction. Filter the filter residue; weigh 10 g of the filter residue obtained above and put it into a 250 mL flask, add 40 mL of sodium hydroxide solution with a concentration of 0.2 mol / L, put it in an ice-water bath, and stir it with a glass rod at 10°C for 10 minutes; after the stirring is completed 15mL of sodium nitrite solution with a mass concentration of 35% was added dropwise to the flask, and then 30mL of a concentrated nitric acid solution ...

example 2

[0018] Add 13mL of m-aminobenzoic acid with a concentration of 0.1mol / L to a 250mL round-bottom flask, then add 60mL of anhydrous ether, place it on a magnetic stirrer, and stir at a speed of 350r / min for 15min to fully dissolve it; keep the magnetic stirring speed While stirring, chlorine gas was introduced into the flask at a rate of 15mL / min, 15mL was ventilated, the shaking table was shaken for 35min, and then 105mL of deionized water was added, stirring was continued for 15min, and the mixture was put into a Buchner funnel for pumping. Filter the filter residue; weigh 15g of the filter residue obtained above and put it into a 250mL flask, add 50mL of sodium hydroxide solution with a concentration of 0.2mol / L, put it in an ice-water bath, and stir it with a glass rod at 13°C for 13min; after the stirring is completed 18mL of sodium nitrite solution with a mass concentration of 35% was added dropwise to the flask, and then 35mL of a concentrated nitric acid solution with a m...

example 3

[0020] Add 15mL of m-aminobenzoic acid with a concentration of 0.1mol / L to a 250mL round-bottom flask, then add 70mL of anhydrous ether, place it on a magnetic stirrer, and stir at a speed of 400r / min for 20min to fully dissolve it; keep the magnetic stirring speed While stirring, chlorine gas was introduced into the flask at a rate of 20mL / min, 20mL was ventilated, the shaking table was shaken for 40min, then 110mL of deionized water was added, stirring was continued for 20min, and the mixture was put into a Buchner funnel for pumping. Filter the filter residue; weigh 20g of the filter residue obtained above and put it into a 250mL flask, add 60mL of sodium hydroxide solution with a concentration of 0.2mol / L, put it in an ice-water bath, and stir it with a glass rod at 15°C for 20min; after the stirring is completed , add dropwise 20mL of sodium nitrite solution with a mass concentration of 35% into the flask, and then dropwise add 40mL of a concentrated nitric acid solution w...

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Abstract

The invention relates to a synthetic method of a compound and in particular relates to a synthetic method of 2,4,6-trichloro-3-nitrobenzoic acid. The method is characterized by taking m-aminobenzoic acid as a raw material and synthesizing 2,4,6-trichloro-3-nitrobenzoic acid through three steps of chlorination, diazotization and hydrolysis. The synthetic method has the advantages of mild reaction conditions and high yield.

Description

technical field [0001] The invention relates to a compound synthesis method, in particular to a synthesis method of 2,4,6-trichloro-3-nitrobenzoic acid. Background technique [0002] 2,4,6-Trichloro-3-nitrobenzoic acid is an organic chemical intermediate, which is widely used in the synthesis of chromogens and has a wide range of uses. There are dozens of varieties of chromogens synthesized with it. Chromogen has unique functions, and is a promising chromogen and synthetic chromogen intermediate, but 2,4,6-trichloro-3-nitrobenzoic acid has never been ideal for industrial production method. The traditional production process of 2,4,6-trichloro-3-nitrobenzoic acid is backward, long process, low yield, large amount of three wastes, and difficult to treat. Contents of the invention [0003] The invention provides a method for synthesizing 2,4,6-trichloro-3-nitrobenzoic acid with mild reaction conditions and high yield. [0004] For achieving the above object, the synthetic ...

Claims

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Application Information

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IPC IPC(8): C07C201/10C07C205/58
CPCC07C201/10C07C227/16C07C245/20C07C205/58C07C229/60
Inventor 陈兴权
Owner CHANGZHOU UNIV
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