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A kind of recrystallization method that improves finasteride purity

A finasteride and recrystallization technology, which is applied in the field of recrystallization to improve the purity of finasteride, can solve problems such as relatively difficult removal, achieve the effects of increasing product competitiveness, mild reaction conditions, and improving drug safety

Active Publication Date: 2020-11-10
TOPFOND PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to the existing production process, the prepared finasteride products can basically meet this standard, but there is greater difficulty in removing impurities І in the existing preparation process, so in terms of improving product quality, it is difficult for the existing production process , especially the purification process still has a lot of room for improvement

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The specific operation of the recrystallization method for improving the purity of finasteride provided in this example is as follows.

[0019] (1) To prepare the crude product solution, take the crude product of finasteride prepared by the prior art (provided by Tianfang Pharmaceutical Co., Ltd., 0.4% single impurity, 0.9% total impurity, impurity І (N-tert-butyl-3-oxo- 4-aza5α-androstane-17β-amide) 0.4%), weighed 50g, placed in a 500mL three-neck flask, added 250mL of water-soluble solvent methanol 5 times the crude product of finasteride, and kept at room temperature ( 25°C) and stir until fully dissolved, add 1.5g of activated carbon (3% by weight of the crude product of finasteride), heat to about 55°C and continue stirring for 10 minutes, filter while hot, rinse with a small amount of methanol, combine the filtrates, and set aside.

[0020] (2) Prepare a crystallization solution, the crystallization solution is phosphoric acid-disodium hydrogen phosphate buffer so...

Embodiment 2

[0025] The specific operation process of the recrystallization method for improving the purity of finasteride provided in this example is the same as in Example 1, and only some parameters are adjusted as follows:

[0026] In step (1), ethanol is used as the water-soluble solvent.

[0027] After testing according to the existing pharmacopoeia testing method, the obtained white crystalline powder of finasteride had a yield of 94.2% and a purity of 99.63%, of which the total impurity was 0.37%, the largest single impurity was 0.10%, and the impurity І was 0.06%.

Embodiment 3

[0029] The specific operation process of the recrystallization method for improving the purity of finasteride provided in this example is the same as in Example 1, and only some parameters are adjusted as follows:

[0030] In step (1), acetone is used as the water-soluble solvent.

[0031] After testing according to the existing pharmacopoeia detection method, the obtained white crystalline powder of finasteride had a yield of 92.9% and a purity of 99.47%, of which the total impurity was 0.53%, the largest single impurity was 0.15%, and the impurity І was 0.09%.

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Abstract

The invention belongs to the technical field of medicine preparation, and particularly relates to a recrystallization method for improving the purity of finasteride in a preparation process of the finasteride. The method comprises the steps of preparing a crude solution, preparing a crystallization solution, carrying out crystallization on the solution, carrying out crystallization and discharging, and the like. According to the invention, a principle that a phosphoric acid-disodium hydrogen phosphate buffering solution is used for recrystallization of dissolved finasteride is adopted to remove impurity I, so that the purity of a finasteride final product is improved. The preliminary effect shows that with the recrystallization method provided by the invention, the yield can reach 90% or above, the yield is high, the total impurities after purification account for less than 0.5%, the maximum individual impurities account for less than 0.2%, the impurities I accounts for less than 0.1%,and all indexes are obviously superior to the current pharmacopeia standard. In conclusion, the recrystallization refining method provided by the application has the advantages of simple related operation, mild reaction conditions and obvious effect of purity improvement, and has good practical value for improving the medicine safety and increasing the product competitiveness.

Description

technical field [0001] The invention belongs to the technical field of medicine preparation, and in particular relates to a recrystallization method for improving the purity of finasteride in the preparation process of finasteride. Background technique [0002] 5α-reductase inhibitors are a class of specific drugs for the treatment of benign prostatic hyperplasia (BPH), and finasteride is a selective but not specific type I and II drug developed by Merck. Type 5α-reductase inhibitors. [0003] Finasteride is the first 5α-reductase inhibitor to be used clinically. Its 5 mg tablet is named Proscar and its 1 mg tablet is named Propecia. The product was approved by the FDA in 1997 for the treatment of male baldness, and can promote hair growth and prevent continued hair loss. [0004] The application results show that high-purity finasteride can reduce the side effects of drugs on patients and improve the quality of life of patients with alopecia. The purity of drugs has a ver...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J73/00
CPCC07J73/005
Inventor 高明王俊臣刘宁宇吉令任真钱丹臧玲陈风殷恒亮杨秋燕杨明张磊陈金春薛娟
Owner TOPFOND PHARMA CO LTD
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