Method for carrying out solvent-out crystallization on allopurinol

A technology of dissolution crystallization and allopurinol, which is applied in the fields of medicine and chemical industry, can solve the problems that the product department is easy to meet the requirements of medicine, low equipment production efficiency, and high organic residue, so as to achieve less solvent residue, good product quality, and increase production Effect

Inactive Publication Date: 2015-03-25
CHONGQING KANGLE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] The technical problem to be solved by the present invention is a dissolution and crystallization method of allopurinol, which solves the common problems in industrial production methods such as cumbersome operation, high energy consumption, low equipment production efficiency, large amount of waste water, high organic residue, and easy access to the product department. Due to defects such as medicinal requirements, the quality index of allopurinol obtained by the method stably meets the requirements of the 2010 edition of "Chinese Pharmacopoeia"

Method used

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  • Method for carrying out solvent-out crystallization on allopurinol
  • Method for carrying out solvent-out crystallization on allopurinol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Add 100 g of crude allopurinol to 1000 g of sulfolane, heat up to 98° C. under stirring to dissolve the material, and obtain a solution. 200 g of purified water was added to the solution for crystallization, and the filter cake was washed twice with 30 g of purified water, sucked dry, and dried at 80°C to obtain 89.2 g of a white crystalline product.

[0036] Experimental results: The HPLC normalization method purity of the product is 99.92%, the yield is 89.2%; the maximum simple impurity content is 0.04%, and other quality indicators meet the requirements of the 2010 edition of "Chinese Pharmacopoeia".

Embodiment 2

[0038] Add 100 g of crude allopurinol to 650 g of sulfolane, heat up to 148° C. under stirring to dissolve the material, and obtain a solution. 200 g of purified water was added to the solution for crystallization, 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.

[0039] Experimental results: The purity of the product by HPLC normalization method is 99.90%, the yield is 89.6%; the maximum simple impurity content is 0.05%, and other quality indicators meet the requirements of the 2010 edition of "Chinese Pharmacopoeia".

Embodiment 3~6

[0041] Based on Example 2, by only changing the consumption of purified water, other conditions are constant (the following table uses "—" to indicate that this condition is the same as Example 2), the results obtained are as follows:

[0042] sequence

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Abstract

The invention provides a method for carrying out solvent-out crystallization on allopurinol. The method comprises the following steps: (1) dissolving a crude allopurinol product into a sulfones solvent at the temperature of 98-148 DEG C; (2) adding a solution obtained from the step (1) to an antisolvent for crystallization, and separating to obtain the allopurinol. The finished allopurinol product obtained through the method provided by the invention can achieve the yield as high as 95% or more than 95% and achieve the purity more than 99.88% of the purity achieved through an HPLC normalization method. The method provided by the invention has the advantages of simple process, small occupied equipment size, output increase of equipment with same size, solvent recycling, environmental pollution reduction and suitability for industrialized production.

Description

technical field [0001] The invention belongs to the technical fields of medicine and chemical industry, and in particular relates to a method for dissolution and crystallization of 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, the chemical structural formula 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 the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/04
CPCC07D487/04
Inventor 李锡伦葛晓强丁瑞陈林杨继斌蔡中文查正华王亚川
Owner CHONGQING KANGLE PHARMA
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