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Synthesis method of 2-hydroxyl-4-bromobenzoic acid

A technology of bromobenzoic acid and a synthetic method is applied in the synthesis field of 2-hydroxy-4-bromobenzoic acid, can solve problems such as high cost, low production capacity, environmental pollution, etc., and achieves simple operation, improved product yield and purity , the effect of easy operation

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

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Problems solved by technology

[0004] The technical problem mainly solved by the present invention: in the process of synthesizing p-bromobenzoic acid at present, adopt the traditional chemical oxidation method to run expensively, cause serious environmental pollution, relatively low production capacity, and the problem that the operation of indirect electrooxidation method is relatively complicated , provides a kind of synthetic method of 2-hydroxyl-4-bromobenzoic acid

Method used

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  • Synthesis method of 2-hydroxyl-4-bromobenzoic acid

Examples

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example 1

[0019] First get 60g of phenol and put it into a 500mL three-neck flask equipped with a stirrer, a thermometer and a dropping funnel, add 50mL of nitric acid with a mass fraction of 69%, control the rotating speed at 500r / min, and stir at a temperature of 10°C. During the stirring process, slowly add 30mL of sulfuric acid with a mass fraction of 75% dropwise, and control the dropwise addition within 15min. After the dropwise addition is completed, raise the temperature to 20°C and set the pressure to 1MPa, and react for 40min to obtain 2-nitro Phenol; then the 2-nitrophenol obtained above is placed in a reaction kettle, 15 mL of hydrogen chloride with a mass fraction of 30% is added thereto, after stirring evenly, after adding 0.5 g of zinc powder, at a temperature of 60 ° C, a pressure Under the condition of 0.8MPa, hydrogen gas was introduced, and the reactor was sealed, and the reaction was continued for 1h to obtain 2-aminophenol; then 10mL of CH with a mass fraction of 37%...

example 2

[0022] First get 100ml of phenol and put it into a 500mL three-necked flask equipped with a stirrer, a thermometer and a dropping funnel, add 55mL of nitric acid with a mass fraction of 69%, control the rotating speed at 550r / min, and stir at a temperature of 13°C. During the stirring process, slowly add 35 mL of sulfuric acid with a mass fraction of 75% dropwise, and control the dropwise addition within 18 minutes. After the dropwise addition is completed, raise the temperature to 23°C and set the pressure at 1.1MPa. React for 43 minutes to obtain 2-nitrate Then put the 2-nitrophenol obtained above in the reaction kettle, add 16mL of hydrogen chloride with a mass fraction of 30% to it, stir evenly, and then add 0.7g of zinc powder, at a temperature of 65°C, Under the condition of a pressure of 1.2MPa, hydrogen gas was introduced, and the reactor was sealed, and the reaction was continued for 1.3h to obtain 2-aminophenol; then 15mL of CH with a mass fraction of 37% was taken 3...

example 3

[0025] First get 120g of phenol and put it into a 500mL three-necked flask equipped with a stirrer, a thermometer and a dropping funnel, add 60mL of nitric acid with a mass fraction of 69% therein, control the rotating speed at 600r / min, and stir at a temperature of 15°C. During the stirring process, slowly add 40mL of sulfuric acid with a mass fraction of 75%, and control the dropwise addition within 20min. After the dropwise addition is completed, raise the temperature to 25°C, set the pressure at 1.2MPa, and react for 45min to obtain 2-nitrate base phenol; then the 2-nitrophenol obtained above is placed in a reaction kettle, 18 mL of hydrogen chloride with a mass fraction of 30% is added thereto, after stirring evenly, after adding 0.8 g of zinc powder, at a temperature of 70 ° C, Under the condition of a pressure of 1.3MPa, hydrogen gas was introduced, and the reactor was sealed, and the reaction was continued for 1.5h to obtain 2-aminophenol; then 18mL of CH with a mass fr...

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Abstract

The present invention discloses a synthesis method of 2-hydroxyl-4-bromobenzoic acid, and belongs to the technical field of organic synthesis. According to the synthesis method disclosed by the present invention, the synthesis method comprises the following steps: using phenol as a raw martial; firstly adding nitric acid and sulfuric acid to generate 2-nitrophenol; then adding HCl and zinc powder to synthesize 2-amino phenol; heating in a water bath and adding CH3COCH to further generate 2-acetamidophenol; next, adding FeBr3 and Br2, and adding CaO2 and triiron tetroxide after the reaction is cooled; and thus generating the 2-hydroxyl-4-bromobenzoic acid disclosed by the present invention after the 2-acetamidophenol is changed into the 2-hydroxyl-4-bromobenzoic acid. The embodiment demonstrates that the synthesis method disclosed by the present invention is not only simple in operation and mild in reaction but also free of pollution, so that the product yield is higher than 89%, and the purity reaches more than 92%.

Description

technical field [0001] The invention discloses a synthesis method of 2-hydroxy-4-bromobenzoic acid, which belongs to the technical field of organic synthesis. Background technique [0002] p-Bromobenzoic acid, also known as 4-bromobenzoic acid, is the most important fine chemical, used in analytical reagents, and is also an intermediate in organic synthesis, used in organic synthesis, and is an intermediate in dyes and medicines. [0003] P-bromobenzoic acid is generally produced through oxidation and acidification. After mixing p-bromotoluene, water, and potassium hydroxide, heat to boil, add potassium permanganate in portions, then reflux for 4 hours, and filter and acidify to obtain the crude product. Then dissolve in dilute ethanol with ammonia water, filter, neutralize with hydrochloric acid, and wash with water to get the finished product. The synthesis methods mainly include chemical oxidation and indirect electro-oxidation. Among them, the chemical oxidation metho...

Claims

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Application Information

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IPC IPC(8): C07C51/16C07C65/05
CPCC07C51/16C07C45/516C07C201/08C07C213/02C07C231/02C07C231/12C07C65/05C07C47/565C07C233/25C07C215/76C07C205/22
Inventor 丁玉琴张帆
Owner 丁玉琴
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