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Synthesis method of 2-chloro-6-bromo-p-nitrobenzoic acid

A technology of p-nitrobenzoic acid and ethyl nitrobenzoate, applied in the field of synthesis of 2-chloro-6-bromo p-nitrobenzoic acid, can solve problems such as expensive formic acid

Inactive Publication Date: 2016-03-23
丁玉琴
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the raw materials used in method 1 are difficult to buy domestically, the formic acid in method 2 is more expensive, and the formic acid solution purchased needs further processing.

Method used

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  • Synthesis method of 2-chloro-6-bromo-p-nitrobenzoic acid

Examples

Experimental program
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Effect test

example 1

[0019] First, 80 mL of toluene was added to a 500 mL three-necked flask, and 5 mL of sulfuric acid with a mass fraction of 90% and 8 mL of nitric acid with a mass fraction of 65% were slowly added thereto, and the reaction temperature was controlled at 30°C for 20 minutes to obtain p-nitrotoluene. Raise the temperature to 70°C, add 2mL of 20% hydrochloric acid solution dropwise into the three-necked flask, add 0.2g of tin powder and 5mL of 40% sodium hydroxide solution after the dropwise addition, stir evenly and react for 20min. To obtain p-toluidine; add 50mL of water, 0.1g of zinc powder, zeolite and 30mL of glacial acetic acid to the obtained p-toluidine, stir evenly, heat in a water bath to 100°C, and react for 40min, add 5mL of acetic anhydride, and the When the white mist stops adding heating, slowly pour the reactant in the beaker into 70mL of cold water under stirring while it is hot, and keep stirring, then perform suction filtration to obtain p-methylacetanilide; add...

example 2

[0021]First, take 90mL of toluene and add it to a 500mL three-neck flask, slowly add 5.5mL of sulfuric acid with a mass fraction of 92% and 9mL of nitric acid with a mass fraction of 68% respectively, and control the reaction temperature at 35°C for 25 minutes to obtain p-nitrotoluene , raise the temperature to 75°C, add 2.5mL hydrochloric acid solution with a mass fraction of 25% to the three-necked flask dropwise, add 0.3g tin powder and 5.5mL sodium hydroxide solution with a mass fraction of 45% after the dropwise addition, and stir to react for 25min , to obtain p-toluidine; add 55mL of water, 0.15g of zinc powder, zeolite and 40mL of glacial acetic acid to the obtained p-toluidine, stir well and then heat it in a water bath to 103°C. After reacting for 45min, add 8mL of acetic anhydride, and When white mist appears in the beaker, stop adding heating, slowly pour the reactant into 75mL of cold water under stirring in the beaker while it is hot, and keep stirring, then carry...

example 3

[0023] First, 100 mL of toluene was added to a 500 mL three-necked flask, and 6 mL of sulfuric acid with a mass fraction of 94% and 10 mL of nitric acid with a mass fraction of 70% were slowly added thereto, and the reaction temperature was controlled at 40°C for 30 minutes to obtain p-nitrotoluene. Raise the temperature to 80°C, drop 3mL of 30% hydrochloric acid solution into the three-necked flask with a straw, add 0.4g of tin powder and 6mL of 50% sodium hydroxide solution after the dropwise addition, stir evenly and react for 30min. To obtain p-toluidine; add 60mL of water, 0.2g of zinc powder, zeolite and 50mL of glacial acetic acid to the obtained p-toluidine, stir evenly and heat it in a water bath to 105°C. After reacting for 50min, add 10mL of acetic anhydride, and the When the white mist stops adding heating, slowly pour the reactant into 80mL of cold water under stirring in the beaker while it is hot, and keep stirring, then carry out suction filtration to obtain p-m...

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Abstract

The present invention discloses a synthesis method of 2-chloro-6-bromo-p-nitrobenzoic acid, and belongs to the field of chemical synthesis. The synthesis method comprises the following steps: firstly using toluene as a raw material to produce p-nitrotoluene; then adding hydrochloric acid and tin powder to obtain p-toluidine; stirring the p-toluidine, the tin powder, zeolite and acetic acid for reaction; adding acetic anhydride after the reaction to produce methylacetanilid; after the production, adding potassium permanganate solution and ethanol for boiling and filtering; adjusting the pH by using a sulfuric acid to obtain p-nitro-ethyl benzoate; heating the obtained p-nitro-ethyl benzoate solid until melting; introducing a chlorine gas to obtain 2,6-dichloro-ethyl p-nitrobenzoate, water, BaBrO3 and dibromomethane; brominating hydrogen with stirring; extracting an organic phase by distillation crystallization to obtain 2-chloro-6-bromo-p-nitro-ethyl benzoate; finally hydrolyzing to obtain the 2-chloro-6-bromo-p-nitrobenzoic acid.

Description

technical field [0001] The invention discloses a synthesis method of 2-chloro-6-bromo-p-nitrobenzoic acid, which belongs to the field of chemical synthesis. Background technique [0002] p-Nitrobenzoic acid is a yellow crystalline powder, odorless and capable of sublimation. Slightly soluble in water, soluble in organic solvents such as ethanol. Combustible in case of open flame and high heat. Thermal decomposition. It is an intermediate used in organic synthesis of medicine, dyestuff, veterinary drug, photosensitive material, etc. It can be obtained by oxidation of p-nitrotoluene. p-Nitrobenzoic acid is an important organic synthesis intermediate and related raw materials, widely used in the production of medicines, pesticides, dyes, etc. The traditional synthesis methods mostly use sodium dichromate and potassium permanganate oxidation, and the reaction can be However, it will generate a lot of toxic waste and pollute the environment. [0003] 2-Amino-5-nitrobenzoic a...

Claims

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Application Information

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IPC IPC(8): C07C201/12C07C205/58
CPCC07C201/12C07C201/08C07C209/36C07C231/02
Inventor 丁玉琴王志慧
Owner 丁玉琴
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