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Industrial production method of m-phthalic acid derivatives

A technology of potassium formate and potassium carbonate, which is applied in chemical instruments and methods, preparation of organic compounds, cyanide reaction preparation, etc., can solve the problems of limiting production efficiency and scale, consuming energy, and being uneconomical, so as to save costs and shorten production time. Response time, the effect of simple production equipment

Active Publication Date: 2015-02-25
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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  • Industrial production method of m-phthalic acid derivatives
  • Industrial production method of m-phthalic acid derivatives
  • Industrial production method of m-phthalic 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, and mix them evenly. After replacing with CO2 gas twice, continue to pass CO2 under 1bar pressure to heat the reaction system To 190-195°C, potassium formate melts completely, and react 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 stratification, discard the organic phase, adjust the aqueous phase to acidity with 1M dilute hydrochloric acid, precipitate solids, filter and dry , 38.0 g of 4-amino-6-hydroxy-isophthalic acid was obtained.

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, and mix them evenly. After replacing with CO2 gas twice, continue to pass it under 1bar pressure 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 stratification, discard the organic phase, adjust the aqueous 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, and mix them evenly. After replacing with CO2 gas twice, continue to flow under 1bar pressure 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 stratification, discard the organic phase, adjust the aqueous 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

The invention discloses an industrial production method of a compound represented by the formula I. The method comprises the following steps: taking p-aminosalicylic acid, potassium salts, and carbon dioxide as the raw materials, and carrying out reactions in melted potassium formate so as to introduce carboxyl groups into a multi-substituted benzene ring under mild conditions. Compared to the prior art, the provided method is carried out under a normal pressure, thus the production operation is safe, furthermore, pricy high-pressure reactor is not required, and the cost is reduced. While the reaction pressure is reduced, the reaction time is not increased, and the reaction time is greatly reduced instead.

Description

Technical field [0001] The invention belongs to a chemical synthesis method of isophthalic acid derivatives, and particularly relates to a method for industrially producing 4-amino-6-hydroxy-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, and the two carboxyl groups are in the meta position. [0003] In the prior art, the compound of formula I can be obtained by using p-aminosalicylic acid of formula II as a raw material and introducing another carboxyl group on its benzene ring. [0004] [0005] However, the carboxylation reaction on the benzene ring is not easy to proceed. Except for some relatively simple substances such as units or polyphenols that can be reacted under low or normal pressure, they generally need to be successful under very high pressure. If there are...

Claims

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Application Information

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IPC IPC(8): C07C229/64C07C227/18
Inventor 许华侨邓青均刘德钦
Owner CHONGQING HUAPONT PHARMA
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