A kind of preparation method of sulfasalazine

A technology of sulfasalazine and sulfasalazine, which is applied in the field of sulfasalazine, can solve the problems of unsatisfactory product purity, difficult synthesis, and few sources, and achieve the effects of large industrial production value, guaranteed yield, and high side reactions

Active Publication Date: 2020-12-29
SUZHOU HUANGHE PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The starting material 4-(4-acetoxy group-3-carbonylmethoxyphenyl azo)-benzenesulfonyl chloride of this method is not commercially available at present and the comparatively difficult method of synthesis, and source is less; In addition, this method is owing to existence Hydrolysis reaction, its yield and product purity are not ideal

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  • A kind of preparation method of sulfasalazine
  • A kind of preparation method of sulfasalazine
  • A kind of preparation method of sulfasalazine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Put sulfapyridine and hydrochloric acid with a substance quantity of 3 in the reaction flask (taking the substance quantity of sulfapyridine as 1), and stir to dissolve it. Control the temperature to 0° C., start to drop the aqueous solution configured by sodium nitrite (the amount of sulfapyridine is 1) with a substance quantity of 1.14, and make it react for 30 minutes to obtain a solution containing a diazonium salt intermediate. Name it A.

[0036] Put salicylic acid and partial sodium hydroxide (taking the amount of sulfapyridine as 1) in the reaction bottle. After the temperature was controlled to 5°C, the above-mentioned A was slowly started to be dropped into the above-mentioned reaction flask, and at the same time, the remaining sodium hydroxide solution was added dropwise to control the pH value of the reaction solution to 10 to start the reaction. The consumption of this sodium hydroxide is 2 (the substance amount of sulfapyridine is 1). After reacting for ...

Embodiment 2

[0040] Put sulfapyridine and hydrochloric acid with a substance quantity of 5 in the reaction flask (taking the substance quantity of sulfapyridine as 1), and stir to dissolve it. The temperature was controlled to 5°C, and the aqueous solution configured by sodium nitrite (with the amount of sulfapyridine being 1) with a substance quantity of 1.06 was started to be added dropwise, and reacted for 15 minutes to obtain a solution containing a diazonium salt intermediate. Name it A.

[0041] Put salicylic acid and partial sodium hydroxide (taking the amount of sulfapyridine as 1) in the reaction bottle. After the temperature was controlled to 10°C, the above-mentioned A was slowly started to be dropped into the above-mentioned reaction flask, and at the same time, the remaining sodium hydroxide solution was added dropwise to control the pH of the reaction solution to 11 to start the reaction. The consumption of this sodium hydroxide is 6 (according to the material quantity of su...

Embodiment 3

[0045]Put sulfapyridine and hydrochloric acid with a substance quantity of 4 in the reaction flask (taking the substance quantity of sulfapyridine as 1), and stir to dissolve it. Control the temperature to 5° C., start to drop the aqueous solution configured by sodium nitrite (with the substance quantity of sulfapyridine as 1) with a substance quantity of 1.10, and make it react for 30 minutes to obtain a solution containing a diazonium salt intermediate. Name it A.

[0046] Put salicylic acid and partial sodium hydroxide (taking the amount of sulfapyridine as 1) in the reaction bottle. After the temperature was controlled to 7°C, the above-mentioned A was slowly started to be dropped into the above-mentioned reaction flask, and at the same time, the remaining sodium hydroxide solution was added dropwise to control the pH of the reaction solution to 10.5 to start the reaction. The consumption of this sodium hydroxide is 4 (according to the substance amount of sulfapyridine is...

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Abstract

The invention discloses a preparation method for sulfasalazine. The preparation method comprises the steps of: S1, carrying out a diazotization reaction on sulfapyridine in an aqueous solution dissolved with hydrochloric acid and sodium nitrite to obtain diazonium salt; S2, carrying out a coupling reaction on the diazonium salt and salicylic acid in a sodium hydroxide aqueous solution to obtain a sulfasalazine crude product; and S3, purifying the sulfasalazine crude product. According to the preparation method disclosed by the invention, by taking sulfapyridine as an initial raw material, the diazotization reaction, the coupling reaction and purification are successively carried out to obtain the sulfasalazine. The diazotization reaction and the coupling reaction have a relatively high conversation rate and relatively few side reactions, so that the purity of the product is improved, and the yield is ensured. In addition, the sulfapyridine is easily available in source, so that the production cost is lowered, and the preparation method has relatively great industrial production value.

Description

technical field [0001] The invention relates to the technical field of sulfasalazine, in particular to a synthesis method of sulfasalazine. Background technique [0002] Sulfasalazine (SASP), also known as 5-[p-(2-pyridinesulfamoyl)benzene]azosalicylic acid. Molecular formula is C 18 h 14 N 4 o 5 S, molecular weight: 398.39. Its molecular structural formula is as follows: [0003] [0004] SASP is mainly used for the treatment of non-specific ulcerative colitis. This product has a special affinity for connective tissue and plays a therapeutic role by releasing sulfapyridine and 5-aminosalicylic acid in the intestinal wall. It is also used clinically for the treatment of rheumatic joints inflammation. Although this product is an old product, the market demand is still very large, especially its quality requirements are getting higher and higher. [0005] In the prior art, there are few disclosures on its preparation method. British Patent GB 11296655 discloses a s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/76
CPCC07D213/76
Inventor 苏子钦徐伏彪江尔胜
Owner SUZHOU HUANGHE PHARMA CO LTD
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