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Preparation, refining method and freeze-drying preparation of injection-grade acetazolamide sodium

A technology of acetazolamide sodium and acetazolamide base, which is applied in the field of injection-grade raw materials of acetazolamide sodium, can solve the problems that the physical and chemical properties have not been studied in detail, there are no literature reports, and it is difficult to remove. Industrial production, low price, easy to control the effect

Active Publication Date: 2013-09-25
ANHUI PIOM PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During the actual operation, we found many problems. First, acetazolamide is almost insoluble in cold water and hot water. In the process of concentrated preparation, acetazolamide produces two new degradation impurities, both of which exceed 0.3%; 2. The impurities of the acetazolamide raw material drug itself are difficult to remove by recrystallization, because acetazolamide is almost insoluble in ethanol, methanol and acetone, and it is difficult to remove acetazolamide that can meet the pharmaceutical standard for crystallization impurities of other solvents
[0017] Regarding the synthesis and refining of acetazolamide sodium, there is no literature report, and its physical and chemical properties have not been studied in detail.

Method used

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  • Preparation, refining method and freeze-drying preparation of injection-grade acetazolamide sodium
  • Preparation, refining method and freeze-drying preparation of injection-grade acetazolamide sodium
  • Preparation, refining method and freeze-drying preparation of injection-grade acetazolamide sodium

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Embodiment 1

[0045]Add 10L of 1M sodium hydroxide solution to a 50L dry and clean reaction kettle, raise the temperature to 30-40°C, add 5.8kg of commercially available acetazolamide under stirring, and adjust the pH to 10-11 with 2M sodium hydroxide solution. , add 30L of acetone, stir for 20min, cool to 5-10°C, precipitate crystals, filter, wash the solid with acetone, and dry in vacuum at 30-40°C for 24h to obtain 6.02kg with a yield of 94.0%.

Embodiment 2

[0047] Add 10L of 1M sodium hydroxide solution to a 50L dry and clean reaction kettle, raise the temperature to 30-40°C, add 5.8kg of commercially available acetazolamide under stirring, and adjust the pH to 10-11 with 2M sodium hydroxide solution. , add 30L of acetone, stir for 20min, cool to 5-10°C, precipitate crystals, filter, wash the solid with acetone, and dry in vacuum at 30-40°C for 24h to obtain 6.12kg with a yield of 95.6%.

Embodiment 3

[0049] In a 30L dry and clean reaction kettle, add 6kg of self-made acetazolamide sodium and 35L of 65% acetone aqueous solution, stir and heat to 45°C, add 52g of injection-grade activated carbon for needles, heat to reflux for 30min, first coarsely filter, and then use 0.22μm micro Filter through a pore filter, put it into the fine drying bag workshop, crystallize, filter, wash the solid with acetone, and dry it under vacuum at 30-40°C for 24 hours to obtain 5.58kg, with a yield of 93.0%.

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Abstract

The invention belongs to the field of chemical preparation and refining methods and products, and in particular relates to a preparation method, a refining method, a freeze-drying product and applications of acetazolamide sodium injection-grade raw material medicine. The preparation method of the injection-grade acetazolamide sodium is characterized in that acetazolamide is dissolved in a dilute alkali solution, a proper amount of an organic solvent is added for crystallization and filtration to obtain a crude product, the crude product is refined through use of a 60%-70% acetone aqueous solution and activated carbon to obtain the injection-grade acetazolamide sodium. The prepared acetazolamide sodium is characterized in that: impurity D is <=0.02%, impurity F is <= 0.01%, impurity A, impurity B, impurity C, and impurity E are not detected, and the purity is higher than 99.99%.

Description

technical field [0001] The invention belongs to the field of chemical preparation and refining methods and products, and more specifically relates to an injection-grade bulk drug of acetazolamide sodium [0002] Preparation method, refining method and freeze-dried product. Background technique [0003] The basic information of acetazolamide sodium is as follows: [0004] Chinese name: Acetazolamide Sodium [0005] English name: Acetazolamide Sodium [0006] Pinyin name: Yixianzuoan Na [0007] Chinese chemical name: N-(5-sulfamoyl-1,3,4-thiadiazol-2-yl)acetamide monosodium salt [0008] English chemical name: N-(5-Sulfamoyl-1,3,4-thiadiazol-2-yl)-acetamide monosodium salt [0009] structural formula [0010] [0011] Molecular formula: C 4 h 5 N 4 NaO 3 S 2 [0012] Relative molecular mass: 244.23 [0013] This product is white or off-white crystalline powder; odorless, slightly bitter taste [0014] Acetazolamide is a heterocyclic sulfonamide carbonic anhyd...

Claims

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Application Information

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IPC IPC(8): C07D285/135A61K31/433A61K9/19A61P43/00A61P9/00A61P35/00
Inventor 徐奎陈正皓魏伟叶加久
Owner ANHUI PIOM PHARMA