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Preparation method of p-aminosalicylic acid

A technology of p-aminosalicylic acid and sodium aminosalicylic acid, applied in the field of preparation of p-aminosalicylic acid, can solve the problems of decreased yield, decreased purity of aminosalicylic acid, generation of impurities, etc., and can reduce drying and heating less time, fewer process steps and higher yield

Pending Publication Date: 2020-10-30
广药白云山化学制药(珠海)有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In the above two patents, the preparation of aminosalicylic acid requires heating, which will lead to the formation of impurities and the decrease of the purity of aminosalicylic acid, and two or more steps are required to prepare aminosalicylic acid. cause a drop in productivity

Method used

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  • Preparation method of p-aminosalicylic acid
  • Preparation method of p-aminosalicylic acid
  • Preparation method of p-aminosalicylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A preparation method of p-aminosalicylic acid, comprising:

[0026] Add sodium p-aminosalicylate dihydrate into the mixed phase of water and organic solvent, the organic solvent includes lower alcohol; add acid solution to adjust pH=2.5-4.0, filter, wash and dry.

[0027] Specifically: sodium p-aminosalicylate dihydrate is added into the mixed phase of water and organic solvent, and the organic solvent includes lower alcohol. Preferably, antioxidants and complexing agents are added to the mixed phase and stirred for 10-30 minutes. The resulting system can be a solid-liquid coexistence, or a clear liquid phase, without complete dissolution. Add acid solution to adjust pH=2.5-4.0; filter, wash and dry to obtain p-aminosalicylic acid.

[0028] Specific steps are as follows:

[0029] Measure water and organic solvent separately and mix.

[0030] Wherein, the water may be selected from drinking water, purified water or water for injection, preferably purified water. Whe...

Embodiment 2

[0038] The present invention provides a method for preparing p-aminosalicylic acid. The method in Example 2 is basically the same as the method in Example 1, the difference mainly lies in the type of organic solvent and the ratio of different types of organic solvents in the organic solvent.

[0039] Adding sodium p-aminosalicylate dihydrate into the mixed phase of water and organic solvents, the organic solvents include lower alcohols and esters; adding acid solution to adjust pH=2.5-4.0, filtering, washing and drying.

[0040] Specifically: sodium p-aminosalicylate dihydrate is added to the mixed phase of water and organic solvents, and the organic solvents include lower alcohols and esters. Preferably, antioxidants and complexing agents are added to the mixed phase and stirred for 10-30 minutes. The resulting system can be a solid-liquid coexistence, or a clear liquid phase, without complete dissolution. Add acid solution to adjust pH=2.5-4.0; filter, wash and dry to obtai...

Embodiment 3

[0050] Add 200mL of water, 200mL of ethanol and 20mL of ethyl acetate into a clean reaction bottle, stir, add 100g of sodium p-aminosalicylate dihydrate, about 0.5g of EDTA, and about 0.5g of sodium sulfite, and stir to dissolve. Add acid solution dropwise, adjust pH=3.5, and stir for 5-10 minutes. Re-measure the pH and control the pH to 3.0. Filter, wash, filter and dry to obtain p-aminosalicylic acid, the purity of the obtained p-aminosalicylic acid is 99.9%, and the yield is 95.2%.

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Abstract

A preparation method of p-aminosalicylic acid comprises the following steps: adding sodium p-aminosalicylate dihydrate into a mixed phase of water and an organic solvent, wherein the organic solvent comprises lower alcohol; and adding an antioxidant and a complexing agent, stirring, adding an acid solution to adjust the pH value to 2.5-4.0, filtering, washing and drying. According to the preparation method of the p-aminosalicylic acid, the sodium p-aminosalicylate dihydrate is taken as a raw material, the sodium salt is converted into organic acid by adding acid, and the water and the mixed organic solvent are taken as solvents, so that a high-density crystal habit and high-purity product is favorably generated, the suction filtration and drying time of the product is shortened, and the preparation efficiency of the product is improved; the p-aminosalicylic acid is prepared by a one-step method, the process steps are few, and the yield is high; and heating is not needed in the whole process to avoid heating oxidation of the p-aminosalicylic acid to generate impurities.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, and in particular relates to a preparation method of p-aminosalicylic acid. Background technique [0002] Palsoniazid, also known as isoniazid p-aminosalicylate, is used to treat various types of pulmonary tuberculosis, endobronchial tuberculosis and extrapulmonary tuberculosis. Palsoniazid is an anti-tuberculosis drug synthesized from p-aminosalicylic acid and isoniazid, and p-aminosalicylic acid is an important intermediate for the preparation of personiazid. In order to prepare high-quality p-aminosalicylic acid, the prior art generally prepares p-aminosalicylic acid first, and then refines it. [0003] Chinese patent CN104402749B neutralizes commercially available sodium p-aminosalicylate dihydrate with sulfuric acid to obtain p-aminosalicylic acid, and then mixes the obtained p-aminosalicylic acid with an organic solvent for refining and fully dissolves to obtain p-aminosalicylic acid . ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/64C07C227/18C07C227/40C07C227/44
CPCC07C227/18C07C227/40C07C227/44C07C229/64
Inventor 金国有
Owner 广药白云山化学制药(珠海)有限公司
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