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Refinasteride refining method, finasteride preparation and preparation method of finasteride preparation

A technology of finasteride and its refining method, which is applied in the direction of non-active ingredient medical preparations, medical preparations containing active ingredients, pill delivery, etc. It can solve the problems of harmfulness to human health, no therapeutic effect, influence on drug stability, Efficacy and other issues to achieve the effect of improving safety, eliminating potential safety hazards, and simple operation

Pending Publication Date: 2022-03-22
湖南醇健制药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The presence of drug impurities in drugs not only has no therapeutic effect, but may also affect the stability and curative effect of drugs, and even be harmful to human health.

Method used

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  • Refinasteride refining method, finasteride preparation and preparation method of finasteride preparation
  • Refinasteride refining method, finasteride preparation and preparation method of finasteride preparation
  • Refinasteride refining method, finasteride preparation and preparation method of finasteride preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] A method for refining finasteride, comprising the steps of:

[0049] With 5g compound finasteride crude product (made by iodination, deiodination route, chromatographic detection such as Figure 5 , according to the area normalization method to calculate the content of 0.169%, chromatographic conditions see later) dissolved in 40g concentrated hydrochloric acid (concentration is 36% ~ 38%), temperature control 25 ℃ dropwise sodium hydroxide aqueous solution (11g sodium hydroxide solution (30 g of water), after the dropwise addition, keep stirring for 10 minutes, filter under reduced pressure, rinse the filter cake with water until it becomes neutral, and dry it with blast at 50°C to obtain the refined finasteride raw material with a yield of 96.7%.

[0050] The content of epoxy impurities contained in the finasteride bulk drug obtained in the present embodiment is detected by high performance liquid chromatography analysis method, and the specific steps are as follows: ...

Embodiment 2

[0066] A method for refining finasteride, comprising the steps of:

[0067] 5g compound finasteride crude product (same as Example 1) was dissolved in 50g concentrated hydrochloric acid (concentration is 36%~38%), and temperature control 30 ℃ was added dropwise sodium hydroxide aqueous solution (13g sodium hydroxide was dissolved in 40g water ), after the dropwise addition was completed, it was incubated and stirred for 10 min, filtered under reduced pressure, the filter cake was rinsed with water until neutral, and dried at 50° C. to obtain refined finasteride bulk drug with a yield of 96.2%.

[0068] The content of epoxy impurities contained in the finasteride bulk drug obtained in this example was detected (the method is the same as in Example 1), and the content of epoxy impurities was 0.07%.

Embodiment 3

[0070] A method for refining finasteride, comprising the steps of:

[0071] 5g compound finasteride crude product (same as Example 1) is dissolved in 40g concentrated hydrochloric acid (concentration is 36%~38%), and temperature control 20 ℃ is added dropwise sodium hydroxide aqueous solution (8g sodium hydroxide is dissolved in 40g water ), after the dropwise addition was completed, it was incubated and stirred for 10 min, filtered under reduced pressure, the filter cake was rinsed with water until neutral, and dried at 50° C. to obtain refined finasteride bulk drug with a yield of 95.2%.

[0072] The content of epoxy impurities contained in the finasteride bulk drug obtained in this example was detected (the method is the same as in Example 1), and the content of epoxy impurities was 0.03%.

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PUM

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Abstract

The invention discloses a finasteride refining method which comprises the following steps: dissolving a finasteride crude product in concentrated hydrochloric acid, adding alkali to separate out a solid, carrying out solid-liquid separation, and drying to obtain the finasteride. The method is simple to operate and high in yield, 1, 2-epoxy finasteride with genetic toxicity can be removed, the content can be controlled to be not higher than 0.1 wt%, the lowest content can be not higher than 0.01 wt% and is far lower than the pharmacopoeia standard (0.1%), the purity is high, and the safety of the finasteride medicine is greatly improved. The invention further discloses a finasteride preparation, the finasteride preparation comprises the finasteride raw material medicine obtained through the refining method and pharmaceutically acceptable carriers and / or auxiliary materials, the content of 1, 2-epoxy finasteride in the finasteride preparation is not higher than 0.01 wt%, and potential safety hazards caused by long-term taking of the finasteride preparation are eliminated.

Description

technical field [0001] The invention belongs to the technical field of crude drug processing, and in particular relates to a finasteride refining method, a finasteride preparation and a preparation method thereof. Background technique [0002] The chemical name of finasteride is N-tert-butyl-3-oxo-4-aza-5α-androst-1-ene-17β-carboxamide, and its chemical formula is C 23 h 36 N 2 o 2 , is a 4-aza steroid compound, its structural formula is as follows: [0003] [0004] Finasteride, as a competitive intracellular enzyme-type II 5α-reductase inhibitor, can very effectively reduce dihydrotestosterone in the blood and prostate, and has reliable therapeutic effects on benign prostatic hyperplasia and androgenetic alopecia, and is safe and Well tolerated. [0005] In the crude drug process development of this medicine, often adopt the synthetic route of bisamide compound as starting material, concrete route is as follows (the following formula shows two steps of iodination a...

Claims

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Application Information

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IPC IPC(8): C07J73/00A61K31/58A61K9/20A61K47/32A61K47/36A61K47/38A61K47/12A61P17/14A61P13/08
CPCC07J73/005A61K9/2013A61K9/2027A61K9/2054A61K9/2059A61K31/58A61P17/14A61P13/08Y02P20/55
Inventor 戴枫林唐杰蒋胜兰唐小海
Owner 湖南醇健制药科技有限公司