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Synthetic method for pharmaceutical intermediate p-chlorobenzoic acid

A technology of p-chlorobenzoic acid and a synthesis method, which is applied in the field of synthesis of a pharmaceutical intermediate p-chlorobenzoic acid, can solve the problems of complicated process and low final yield, and can reduce intermediate links, shorten reaction time, and improve reaction yield. rate effect

Inactive Publication Date: 2018-10-16
CHENGDU ZHONGHENG HUATIE TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] p-Chlorobenzoic acid is mainly used as an intermediate of medicine, pesticide, dyestuff and organic synthesis. The intermediate of dyestuff and medicine, however, most of the existing synthetic methods adopt p-chlorotoluene as reactant, the process is more complicated, and the final yield is not very high, therefore, it is necessary to propose a new synthetic method, which is useful for further It is of great economic significance to improve the quality and yield of products and reduce the content of by-products

Method used

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  • Synthetic method for pharmaceutical intermediate p-chlorobenzoic acid

Examples

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Effect test

example 1

[0011] Add 3L of 2-chloroethanol solution with a mass fraction of 30% into the reaction vessel, control the stirring speed at 90rpm, add 2mol of benzene solution with a mass fraction of 50%, 3mol of dichloroacetic acid, and 30g of potassium ferricyanide powder, and increase the temperature of the solution to Keep at 70°C for 70 minutes, lower the solution temperature to 10°C, precipitate solids, filter, wash the solids with 60% aniline solution, combine the washing liquid and filtrate, adjust the pH to 2 with 25% oxalic acid solution, and precipitate precipitates , filtered, the solid was washed with 45% potassium nitrate solution by mass fraction, washed by 70% 2-octanol solution by mass fraction, washed by 80% 2-butoxyethanol solution by mass fraction, dehydrated by anhydrous calcium sulfate dehydrating agent , to get 266.22 g of finished p-chlorobenzoic acid, yield 85%.

example 2

[0013] Add 3L of 2-chloroethanol solution with a mass fraction of 35% into the reaction vessel, control the stirring speed at 100rpm, add 2mol mass fraction of 53% benzene solution, 3.5mol of dichloroacetic acid, 30g of potassium ferricyanide powder, and raise the temperature of the solution to 70°C, keep it for 70min, lower the solution temperature to 10°C, precipitate solids, filter, wash the solids with 62% aniline solution, combine the washing liquid and filtrate, adjust the pH to 2.5 with 27% oxalic acid solution, and precipitate Precipitate, filter, wash the solid with 47% potassium nitrate solution, 73% 2-octanol solution, 83% 2-butoxyethanol solution, solid sodium hydroxide dehydrating agent After dehydration, 278.75 g of p-chlorobenzoic acid was obtained, with a yield of 89%.

example 3

[0015] Add 3L of 39% 2-chloroethanol solution into the reaction vessel, control the stirring speed to 110rpm, add 2mol of 57% benzene solution, 4mol of dichloroacetic acid, 40g of potassium ferricyanide powder, and increase the temperature of the solution to Keep at 80°C for 80 minutes, lower the temperature of the solution to 16°C, precipitate solids, filter, wash the solids with 65% aniline solution, combine the washing liquid and filtrate, adjust the pH to 3 with 30% oxalic acid solution, and precipitate precipitates , filtered, the solid was washed with 50% potassium nitrate solution by mass fraction, washed by 76% 2-octanol solution, 87% by 2-butoxyethanol solution, anhydrous calcium sulfate dehydrating agent After dehydration, 288.14 g of p-chlorobenzoic acid was obtained, with a yield of 92%.

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Abstract

The invention discloses a synthetic method for pharmaceutical intermediate p-chlorobenzoic acid. The method mainly comprises the following steps: adding 3 L of a 2-chloroethanol solution into a reaction vessel, controlling a stirring speed to be 90-110 rpm, adding 2 mol of a benzene solution, 3-4 mol of dichloroacetic acid and 30-40 g of potassium ferricyanide powder, heating the solution to temperature of 70-80 DEG C, keeping the temperature for 70-80 min, cooling the solution to temperature of 10-16 DEG C for precipitating a solid, performing filtering, washing the solid by using an anilinesolution, merging the washing liquid and the filtrate, adjusting the pH to 2-3 by using an oxalic acid solution for precipitating a precipitate, performing filtering, washing the solid by using a potassium nitrate solution, performing washing by using a 2-octanol solution, performing washing by using a 2-butoxyethanol solution, and performing dehydration by using a dehydrating agent to obtain thefinished-product p-chlorobenzoic acid.

Description

technical field [0001] The invention relates to a method for synthesizing a pharmaceutical intermediate p-chlorobenzoic acid. Background technique [0002] p-Chlorobenzoic acid is mainly used as an intermediate of medicine, pesticide, dyestuff and organic synthesis. The intermediate of dyestuff and medicine, however, most of the existing synthetic methods adopt p-chlorotoluene as reactant, the process is more complicated, and the final yield is not very high, therefore, it is necessary to propose a new synthetic method, which is useful for further It is of great economic significance to improve the quality and yield of products and reduce the content of by-products. Contents of the invention [0003] The object of the present invention is to provide a kind of synthetic method of medicine intermediate p-chlorobenzoic acid, comprises the steps: [0004] (i) Add 3L of 2-chloroethanol solution into the reaction vessel, control the stirring speed at 90-110rpm, add 2mol of ben...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/353C07C63/70
CPCC07C51/353C07C63/70
Inventor 彭响亮
Owner CHENGDU ZHONGHENG HUATIE TECH CO LTD
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