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Method for industrial production of isophthalic acid derivatives

A technology of potassium formate and potassium carbonate, applied in chemical instruments and methods, preparation of organic compounds, preparation of cyanide reactions, etc., can solve problems such as limiting production efficiency and scale, consuming energy, being uneconomical, etc., and achieving cost saving and shortening. Response time, simple effect of production equipment

Active Publication Date: 2018-03-27
CHONGQING HUAPONT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The disadvantages of carrying out the reaction conditions according to the prior art are: the long-term high-pressure reaction is dangerous, consumes energy, is uneconomical, and limits the production efficiency and scale, so it is difficult to produce under industrialized large-scale conditions

Method used

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  • Method for industrial production of isophthalic acid derivatives
  • Method for industrial production of isophthalic acid derivatives
  • Method for industrial production of isophthalic acid derivatives

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] In a three-necked reaction flask, add 30.6g of p-aminosalicylic acid, 27.6g of potassium carbonate, and 184.9g of potassium formate, mix well, pass CO2 gas replacement twice, continue to pass CO2 under 1 bar pressure, and heat the reaction system At 190-195°C, the potassium formate melts completely, and reacts at this temperature for 2.5 hours. After the reaction is completed, add DMSO to the reaction system, stir to form a slurry, then add water and ethyl acetate for extraction and layering, discard the organic phase, adjust the water phase to acidity with 1M dilute hydrochloric acid, precipitate solids, filter, and dry to obtain 38.0 g of 4-amino-6-hydroxy-isophthalic acid.

Embodiment 2

[0039] In a three-necked reaction flask, add 25.0g of p-aminosalicylic acid, 33.8g of potassium carbonate, 8.1g of potassium bicarbonate, and 26.9g of potassium formate. CO2, heat the reaction system to 185-190°C, the potassium formate is completely melted, and react at this temperature for 3.5 hours. After the reaction is completed, add DMSO to the reaction system, stir to form a slurry, then add water and ethyl acetate for extraction and layering, discard the organic phase, adjust the water phase to acidity with 1M dilute hydrochloric acid, precipitate solids, filter, and dry , 31.0 g of 4-amino-6-hydroxy-isophthalic acid was obtained.

Embodiment 3

[0041] In a three-necked reaction flask, add 20.1g of p-aminosalicylic acid, 35.9g of potassium carbonate, 13.8g of potassium bicarbonate, and 65.9g of potassium formate. CO2, heat the reaction system to 171-178°C, the potassium formate is completely melted, and react at this temperature for 1 hour. After the reaction is completed, add DMSO to the reaction system, stir to form a slurry, then add water and ethyl acetate for extraction and layering, discard the organic phase, adjust the water phase to acidity with 1M dilute hydrochloric acid, precipitate solids, filter, and dry , 24.0 g of 4-amino-6-hydroxy-isophthalic acid was obtained. Example 4

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Abstract

A method for industrial production of formula I, using p-aminosalicylic acid, potassium salt and carbon dioxide as raw materials, the reaction is carried out in molten potassium formate, so that multi-substituted benzene rings can reintroduce carboxyl groups under mild conditions. Compared with the prior art, the present invention reacts under normal pressure, has safe production operation, does not need expensive high-pressure reactors, and saves costs; and while reducing the reaction pressure, it not only does not need to increase the time required for the reaction, but instead Significantly reduced reaction time

Description

technical field [0001] The invention belongs to a chemical synthesis method of isophthalic acid derivatives, in particular to a method for industrialized production of 4-amino-6-hydroxyl-isophthalic acid. Background technique [0002] 4-Amino-6-hydroxy-isophthalic acid (Formula I) is a phthalic acid compound and an important intermediate in pharmaceuticals. In its structure, the benzene ring is four-substituted by carboxyl, amino and hydroxyl groups, and the two carboxyl groups are in the meta position. [0003] In the prior art, the compound of formula I can be obtained from p-aminosalicylic acid of formula II by introducing another carboxyl group into its benzene ring. [0004] [0005] However, the carboxylation reaction on the benzene ring is not easy to carry out. Except for some substances with relatively simple structures, such as unit or polyphenols, which can react under low pressure or normal pressure, they generally need to be successful under very high press...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C229/64C07C227/18
Inventor 许华侨邓青均刘德钦
Owner CHONGQING HUAPONT PHARMA
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