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Purification method of allopurinol

A purification method and technology for allopurinol, applied in the field of purification of allopurinol, can solve the problems affecting product yield, quality, sample destruction, and complicated operation, and achieve the advantages of reducing production cost, improving equipment production capacity and simple process. Effect

Active Publication Date: 2014-07-02
NEW FOUNDER HLDG DEV LLC +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the water consumption of this method is reduced, the operation is cumbersome, and the sample is easily damaged in an over-alkali and over-acid environment, which can affect product yield and quality.

Method used

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  • Purification method of allopurinol
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  • Purification method of allopurinol

Examples

Experimental program
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Effect test

Embodiment 1

[0061] Weigh 100g of the crude product of allopurinol, add 2100g of DMF, heat up to 150°C under stirring to dissolve the material, add 5g of activated carbon, decolorize under stirring for 15 minutes, filter while it is hot, and wash the carbon residue with 50g of DMF; cool the filtrate to room temperature, analyze The crystals were filtered out, and the filter cake was washed twice with 30 g of purified water, sucked dry, and dried at 80° C. to obtain 92.8 g of a white crystalline product.

[0062] Experimental results: the purity of the product is 99.979%, and the yield is 92.8%. The content of the largest single impurity is 0.021%, the content of the total impurities is 0.021%, and other indicators are in line with the pharmacopoeia standards.

Embodiment 2

[0064] Weigh 100g of crude allopurinol, add 600g of DMSO, heat up to 150°C under stirring, dissolve the material, add 5g of activated carbon, decolorize under stirring for 15 minutes, filter while hot, wash the carbon residue with 50g of DMSO, cool the filtrate to room temperature, and crystallize , the crystals were filtered out, and the filter cake was washed twice with 30 g of purified water, sucked dry, and dried at 80° C. to obtain 89.6 g of a white crystalline product.

[0065] Experimental results: the purity of the product is 99.919%, and the yield is 89.6%. The content of the largest single impurity is 0.068%, the content of the total impurity is 0.081%, and other items are in line with the pharmacopoeia standards.

Embodiment 3

[0067] Weigh 100g of crude allopurinol, add 2500g of ethylene glycol, heat up to 150°C under stirring, and dissolve the material, add 10g of activated carbon, decolorize under stirring for 15 minutes, filter while hot, wash the carbon residue with 50g of ethylene glycol, and cool the filtrate Bring to room temperature, crystallize, and filter out the crystals. The filter cake was washed with 30 g of purified water for three times, sucked dry, and dried at 80° C. to obtain 88.2 g of off-white crystalline product.

[0068] Experimental results: the purity of the product is 99.875%, and the yield is 88.2%. The content of the largest single impurity is 0.087%, the content of the total impurities is 0.125%, and other indicators are in line with the pharmacopoeia standards.

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Abstract

The invention provides a purification method of allopurinol. The method provided by the invention comprises the following steps: 1) dissolving an allopurinol crude product in a high-boiling point polar organic solvent at the temperature of 100-190 DEG C; 2) performing decolorization treatment on a solution obtained in the step 1), and filtering when the solution is hot; 3) cooling and devitrifying filtrate obtained in the step 2), and separating to obtain purified allopurinol crystals. By adopting the method provided by the invention, the yield of the obtained allopurinol finished product is high, which can be as high as 90%, and the purity is good, which can be above 99.88%. Furthermore, the method provided by the invention has a simple process, the yield is greatly improved, the solvent can be completely recycled, environmental pollution is reduced, and the method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of pharmacy, and in particular relates to a method for purifying allopurinol. Background technique [0002] Allopurinol is also known as allopurinol, aropurine, allopurinol, cyloryl, hydroxypyrazole pyrimidine, the English name is Allopurinol, and the chemical name is 1H-pyrazolo[3,4-d]pyrimidine-4 Alcohol, molecular formula C 5 h 4 N 4 O, the molecular weight is 136.11, and its chemical structure is as follows: [0003] [0004] Allopurinol is a xanthine oxidase inhibitor, suitable for various diseases with primary or secondary serum uric acid increase, such as gout, acute or chronic leukemia, polycythemia vera, multiple myeloma and other malignant Hyperuricemia caused by massive necrosis of tumor cells during chemotherapy or radiotherapy can prevent and treat urate nephropathy, etc., with remarkable curative effect and minimal side effects, so it is widely used clinically. [0005] The preparation method of ...

Claims

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Application Information

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IPC IPC(8): C07D473/30
CPCC07D487/04
Inventor 马德银马芳邓婕赵德李明川
Owner NEW FOUNDER HLDG DEV LLC
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