A kind of refining method of vidarabine monophosphate

A technology for adenosine monophosphate and crude adenosine monophosphate, which is applied in the field of medicine and chemical industry and can solve the problems of product instability, high temperature, low product purity and yield, etc.

Active Publication Date: 2015-07-29
GUANGDONG XIANQIANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the refining method of vidarabine monophosphate is to dissolve the crude product of vidarabine monophosphate under reflux with water, decolorize activated carbon, filter, and crystallize. The temperature required by this method is too high, and the product is unstable during the production process. By-products, resulting in low product purity and yield

Method used

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  • A kind of refining method of vidarabine monophosphate

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Embodiment 1

[0021] Under the protection of nitrogen, add 20g of vidarabine monophosphate crude product and 1g of sodium sulfite into 200ml of water, adjust the pH to 9.5 with 2N sodium hydroxide solution, heat to 40°C, stir to dissolve, then add 1g of activated carbon, keep warm at 40°C and stir Decolorize, filter while hot, adjust the filtrate to pH = 4 with 2N sulfuric acid solution, cool to -5 ~ 0°C, stir to crystallize, filter, wash with ice water, and dry to obtain 18.4g of refined vidarabine monophosphate, content 99.94%, refined Yield 92%.

Embodiment 2

[0023] Add 20g of vidarabine monophosphate crude product and 1g of ammonium sulfite into 200ml of water, adjust the pH to 10 with 28% ammonia solution, heat to 40°C, stir to dissolve, then add 0.6g of activated carbon, keep warm at 40°C and stir to decolorize. Filter while it is hot, adjust the filtrate to pH=3.5 with 2N hydrochloric acid solution, cool to -5~0°C and stir to crystallize, filter, wash with ice water, and dry to obtain 18.2g of refined vidarabine monophosphate, content 99.95%, refined yield 91%.

Embodiment 3

[0025] Add 20g of vidarabine monophosphate crude product and 1g of sodium sulfite into 400ml of water, adjust the pH to 8 with 2N sodium hydroxide solution, heat to 40°C, stir to dissolve, then add 1g of activated carbon, keep warm at 40°C and stir to decolorize, while hot Filter and adjust the filtrate to pH=5 with 2N sulfuric acid solution, lower the temperature to -5~0°C and stir to crystallize, filter, wash with ice water, and dry to obtain 17.2g of refined vidarabine monophosphate, the content is 99.96%, and the refined yield is 86% .

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Abstract

The invention discloses a refining method of vidarabine monophosphate. The refining method is characterized by comprising the following steps of: regulating the pH of a vidarabine monophosphate crude product and an antioxidant to 8-10 by using alkali, and heating and dissolving; then adding a right amount of active carbon, and filtering while hot; regulating pH to 3-5; and crystallizing. The refining method disclosed by the invention can achieve high yield and can be used for refining the high-purity vidarabine monophosphate.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, and in particular relates to a method for refining vidarabine monophosphate. Background technique [0002] Vidarabine monophosphate (Am-AMP) is the monophosphate compound of vidarabine (Ara-A), and it is a synthetic adenosine antiviral drug. After adenosine monophosphate enters the cell, it undergoes phosphorylation to generate adenosine adenosine diphosphate (Ara-ADP) and adenosine adenosine triphosphate (Ara-ATP). The antiviral activity is mainly caused by adenosine triphosphate (Ara-ATP), which competes with deoxyadenosine triphosphate (dATP) to bind to viral DNAP, thereby inhibiting the activity of enzymes and the synthesis of viral DNA , while inhibiting the activity of viral nucleotide reductase to inhibit the synthesis of viral DNA, it can also inhibit the activity of viral DNA terminal deoxynucleotidyl transferase, so that Ara-A can penetrate into the viral DNA and connect t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H19/20C07H1/06
Inventor 郑玉春张志生孙晔杜丽丽王雪志方谷良武春
Owner GUANGDONG XIANQIANG PHARMA
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