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Preparing method of balsalazide sodium

A technology of balsalazide sodium and balsalazide, which is applied in the field of medicine, can solve the problems that balsalazide sodium does not meet the standards of the United States Pharmacopoeia, and achieve the effects of stable process, high yield and simple operation

Inactive Publication Date: 2019-07-12
赤峰蒙欣药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] U.S. Patent US4412992, British Patent GB208079, Chinese Patent CN101503377A and CN104974061B and other published literature reports, the solvent used for the refining of balsalazide is ethanol or glacial acetic acid solution, and the used solvent for the preparation of balsalazide sodium is ethanol solution. Related substances of balsalazide sodium prepared by the above method do not meet the standards of the United States Pharmacopoeia

Method used

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  • Preparing method of balsalazide sodium

Examples

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Comparison scheme
Effect test

Embodiment 1

[0020] (1) Refining of balsalic acid: Add 100g of crude balsalic acid and 150g of dimethylformamide into a 500ml three-neck round bottom flask, heat to 85°C and stir until the crude balsalic acid is completely dissolved, then add 3g of activated carbon Decolorize for 1 hour, filter with suction; add the filtrate to a 1000ml three-necked round bottom flask, heat to 75°C, add 400g of ethanol, slowly cool down to 30°C, keep warm for 3 hours, continue to cool to 15°C and filter with suction, wash with ethanol, and dry Obtained 91.5g of balsalazide refined product, the purity was 99.4% detected by the USP related substance method, and the largest single impurity was 0.18%.

[0021] (2) Preparation of balsalazide sodium: Add 100g of refined balsalazide and 300g of dimethylformamide into a 500ml three-necked round-bottomed flask, heat to 40°C and stir to completely dissolve the refined balsalazide. Slowly add 25% (W / W) sodium hydroxide solution dropwise at temperature, control the pH...

Embodiment 2

[0023] (1) Refining of balsalic acid: Add 100g of crude balsalic acid and 200g of dimethyl sulfoxide into a 500ml three-neck round bottom flask, heat to 80°C and stir until the crude balsalic acid is completely dissolved, then add 3g of activated carbon Decolorize for 1 hour, filter; add the filtrate to a 2000ml three-neck round bottom flask, heat to 70°C, add 500g of ethanol, slowly cool down to 35°C, keep warm for crystallization for 4 hours, continue cooling to 15°C for suction filtration, wash with ethanol, and dry to obtain 89.1g of balsalazide refined product, with a purity of 99.6% detected by the USP related substance method, and the largest single impurity is 0.12%.

[0024] (2) Preparation of balsalazide sodium: Add 100g of refined balsalazide and 200g of dimethyl sulfoxide into a 500ml three-neck round bottom flask, heat to 50°C and stir to completely dissolve the refined balsalazide. Slowly add 30% (W / W) sodium hydroxide solution dropwise at temperature, control th...

Embodiment 3

[0026] (1) Refining of balsalic acid: Add 100g of crude balsalic acid and 350g of dimethylformamide into a 500ml three-neck round bottom flask, heat to 80°C and stir until the crude balsalic acid is completely dissolved, then add 3g of activated carbon Decolorize for 1 hour, filter; add the filtrate to a 2000ml three-neck round bottom flask, heat to 78°C, add 600g of ethanol, slowly cool down to 40°C, keep warm for crystallization for 4.5 hours, continue cooling to 17°C for suction filtration, wash with ethanol, and dry to obtain 90.7g refined product of balsalazide, the purity of which is 99.5% by USP related substance method, and the largest single impurity is 0.10%.

[0027] (2) Preparation of balsalazide sodium: Add 100g of refined balsalazide and 400g of dimethyl sulfoxide into a 1000ml three-neck round-bottomed flask, heat to 60°C and stir to completely dissolve the refined balsalazide. Slowly add 35% (W / W) sodium hydroxide solution dropwise at high temperature, control ...

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Abstract

The invention discloses a preparing method of balsalazide sodium. The method includes the steps of refining balsalazide acid and preparing the balsalazide sodium. The step of refining the balsalazideacid includes the substeps of dissolving a coarse balsalazide acid product in dimethyl formamide or dimethyl sulfoxide, conducting decoloring, adding ethyl alcohol, and conducting heat preserving, crystallizing, washing and drying to prepare a fine balsalazide acid product. The step of preparing the balsalazide sodium includes the substeps of dissolving the fine balsalazide acid product in dimethyl formamide or dimethyl sulfoxide, dropwise adding a sodium hydroxide solution, dropwise adding ethyl alcohol, and conducting crystallizing, washing and drying to prepare the balsalazide sodium. In the process of refining the balsalazide acid and preparing the balsalazide sodium, the dimethyl formamide or dimethyl sulfoxide is used as the solvent, impurities can be effectively removed, the qualitymeets the requirements of American pharmacopeia standards, and the process is simple and stable.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a preparation method of balsalazide sodium. Background technique [0002] Balsalazide Disodium, the chemical name is (E)-5-[[4-[(2-carboxyethyl)carbamoyl]phenyl]azo]salicylic acid disodium salt dihydrate, CAS number: 80573-04-2. A new type of 5-aminosalicylic acid prodrug listed in the UK by the Swiss company Astra in 1997, the trade name is Coiazide; it was approved for marketing in the United States in 2000. It is used in the treatment of ulcerative colitis, proctitis and Crouse's disease. Because of its fast onset, good curative effect, good tolerance, and small side effects, it is currently an ideal anticolon drug. Its structural formula is: [0003] [0004] Balsalazide sodium is recorded in the Chinese Pharmacopoeia and the United States Pharmacopoeia. The requirements of the relevant substances in the Chinese Pharmacopoeia are that the individual impuri...

Claims

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Application Information

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IPC IPC(8): C07C245/08
CPCC07B2200/13C07C245/08
Inventor 李渤崔晶华林士淇高艳波李晓光
Owner 赤峰蒙欣药业有限公司
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