Production method of balsalazide

A production method and technology of balsalazide, applied in the field of pharmaceutical preparation, can solve the problems of complex manufacturing process, high production cost, poor product quality and the like, and achieve the effects of good product quality and simple manufacturing method

Inactive Publication Date: 2015-07-01
李磊
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the current process of manufacturing balsalazide, the manufacturing proc

Method used

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Embodiment Construction

[0006] Now in conjunction with the present invention for further detailed description.

[0007] A kind of production method of balsalazide of the present invention, concrete steps are as follows: a. Beta-alanine and sodium carbonate are dissolved in water, add triethylbenzyl ammonium chloride, drop the dinitrobenzoyl chloride Chloromethane solution, stirred at room temperature for 3h; standing to separate layers, the aqueous layer was acidified to pH 1 with hydrochloric acid; filtered, dried, and recrystallized from acetone to obtain N-p-nitrobenzoyl-β-alanine; b. Dissolve it in ethanol, add activated palladium for hydrogenation; filter, concentrate, add ether, filter to obtain N-p-aminobenzoyl-β-alanine; c. Add the reduced product to a small amount of Make a paste in concentrated hydrochloric acid, add water to dilute, slowly add sodium nitrite solution, and stir for 1 hour; dropwise add salicylic acid alkali solution, adjust pH to 8.2, and stir for 3 hours; drop the reaction...

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Abstract

The invention relates to a production method of balsalazide, wherein the production method comprises the following specific steps: a, dissolving beta-alanine and sodium carbonate in water, adding benzyltriethylammonium chloride, dropwise adding a dichloromethane solution of p-nitrobenzoyl chloride, and stirring for 3 h at room temperature; allowing to stand for layering, and acidifying the aqueous layer with hydrochloric acid to pH of 1; carrying out acetone recrystallization, to obtain N-p-nitrobenzoyl-beta-alanine; b, dissolving N-p-nitrobenzoyl-beta-alanine in ethanol, adding activated palladium, and carrying out hydrogenation; and adding ethyl ether, filtering, and thus obtaining N-p-aminobenzoyl-beta-alanine; and c, cooling with ice bath, adding a reduction product to a small amount of concentrated hydrochloric acid to form a paste, adding water to dilute, slowly adding a sodium nitrite solution, and stirring for 1 h; dropwise adding an alkaline solution of salicylic acid, adjusting the pH to 8.2, and stirring for 3 h; and dropwise adding the reaction liquid into an ice-dilute hydrochloric acid mixed solution, filtering, drying, carrying out ethanol recrystallization, and thus obtaining the product balsalazide. According to the production method of balsalazide, the production method is simple, and the product quality is good.

Description

technical field [0001] The invention relates to the field of medicine preparation, in particular to a production method of balsalazide. Background technique [0002] Balsalazide is a prodrug of 5-aminosalicylic acid. For the treatment of mildly to moderately active ulcerative colitis. Because currently in the process of manufacturing balsalazide, the manufacturing process is complicated, the production cost is high, and the product quality is poor. Contents of the invention [0003] The technical problem to be solved by the present invention is: in order to overcome the above-mentioned problems, a production method of balsalazide is provided. [0004] The technical scheme that the present invention solves its technical problem is: a kind of production method of balsalazide, concrete steps are as follows: a. beta-alanine and sodium carbonate are dissolved in water, add triethylbenzyl ammonium chloride, Add a dichloromethane solution of p-nitrobenzoyl chloride dropwise, s...

Claims

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Application Information

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IPC IPC(8): C07C245/08
Inventor 李磊
Owner 李磊
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