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After-treatment process for mesalazine crude product

A technology of mesalazine and crude products, which is applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problems of shortening working hours, difficult drying, difficult filtration, etc., to improve quality and purity, reduce drying temperature, The effect of reducing the content of impurities

Active Publication Date: 2019-01-11
HANGZHOU HUANGSEN BIOLOGICAL TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In view of this, the purpose of the present invention is to provide a post-treatment process for crude mesalazine, which solves the defects of difficult filtration and difficult drying in the current production process, not only simplifies the production operation process, shortens the working hours, but also significantly Reduced production energy consumption, suitable for industrialized production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Add 320 g of water, 40 g of crude mesalazine with a content of 99.5%, and 48 g of 30% industrial hydrochloric acid in the reaction flask, stir and heat up to 80° C. to dissolve the system, add 2 g of activated carbon, stir and decolorize for 1 hour, filter while hot, and the filtrate Cool to 50°C, first drop 14g of 10% KH 2 PO 4 After 2 hours of dripping, slender needle-like crystals precipitated, and then continued to add dropwise 30% sodium hydroxide solution to adjust the pH to 3.0, cooled to room temperature, filtered, washed with water, and dried at 50°C for 4 hours to obtain Mesalazine 37.2 g.

[0049] After calculation, the yield of mesalazine: 93%, purity: 99.8%.

Embodiment 2

[0051] Add 320g of water, 40g of crude mesalazine with a content of 99.5%, and 134g of 30% sulfuric acid to the reaction flask, stir and heat up to 90°C to dissolve the system, add 2g of activated carbon, stir and decolorize for 1 hour, filter while it is hot, and cool the filtrate to 60°C, first drop 13.5g of 15% K 2 HPO 4 After 0.5 hours of dripping, elongated needle-like crystals were precipitated, and then continued to add dropwise 30% sodium hydroxide solution to adjust the pH to 4.0, cooled to room temperature, filtered, washed with water, and dried at 60°C for 6 hours to obtain 38g of mesalazine fine product .

[0052] After calculation, the yield of mesalazine: 95%, the purity: 99.9%.

Embodiment 3

[0054] Add 320g, 40g of crude mesalazine with a content of 99.3% and 54g of 35% industrial hydrochloric acid to the reaction flask, stir and heat up to 80°C to dissolve the system, add 2g of activated carbon, stir and decolorize for 1 hour, filter while it is hot, and cool the filtrate to 60°C, first drop 16.5g of 20% K 3 PO 4 After 1.5 hours of dripping, elongated needle-like crystals were precipitated, and the saturated sodium carbonate solution was added dropwise to adjust the pH to 3.0, cooled to room temperature, filtered, washed with water, and dried at 53° C. for 5 hours to obtain 37.6 g of mesalazine fine product.

[0055] After calculation, the yield of mesalazine: 94%, the purity: 99.9%.

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Abstract

The invention provides an after-treatment process for a mesalazine crude product, belonging to the preparation field of mesalazine. According to the after-treatment process, mesalazine is separated ina form of thin and long needle-like crystal by virtue of a buffer solution and is easily filtered, the after-treatment operation is relatively convenient, the drying temperature is reduced, the drying time is shortened, and the production energy consumption is substantially reduced. Meanwhile, mesalazine prepared by virtue of the after-treatment process reaches up to 99.8%-99.9%, the impurity content of a mesalazine fine product is reduced, the appearance color is bright, the yield reaches 91%-95%, and the appearance color is white, the yield reaches 91%-95%, and the after-treatment process meet the demands of industrially produced mesalazine on the purity and the yield.

Description

technical field [0001] The invention relates to the technical field of mesalazine industrialized production, in particular to a post-treatment process for crude mesalazine. technical background [0002] Mesalazine (Mesalazine), the chemical name is 5-aminosalicylic acid (5-ASA), also known as Masalazine, is used for the treatment of mild and moderate ulcerative colitis and the maintenance treatment of ulcerative colitis. Inflammation of the wall was significantly suppressed. Mesalazine can inhibit the synthesis of prostaglandins that can cause inflammation and the formation of inflammatory mediator leukotrienes, thereby significantly inhibiting the inflammation of the intestinal mucosa, and has a better effect on the connective tissue of the inflamed intestinal wall. At present, 5-ASA is widely used clinically and has become the drug of choice for the treatment of inflammatory bowel disease (IBD). [0003] It is known in the prior art that during the crystallization proces...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/42C07C229/64C07C227/40
CPCC07C227/40C07C227/42C07C229/64
Inventor 盛景新黄锋王涛贾春祥
Owner HANGZHOU HUANGSEN BIOLOGICAL TECH CO LTD
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