Purification method of penciclovir

A refining method, the technology of penciclovir, which is applied in the field of compound preparation, can solve problems such as unguaranteed, and achieve the effects of low cost, strong repeatability, and simple operation

Active Publication Date: 2014-10-08
JINAN KANGHE MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The refining method of penciclovir crude product mentioned in the synthesis process of penciclovir announced by WO0006573 and WO9528402A2, it utilizes the different solubility of penciclovir in water under different pH conditions, adopts acid-base method to refine, this refining method can Reduce the content of 9-(4-hydroxy-1-butyl)guanine impurity but cannot guarantee to reduce it below 0.10%

Method used

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  • Purification method of penciclovir
  • Purification method of penciclovir
  • Purification method of penciclovir

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Under stirring, add 40 g of crude penciclovir with 0.41% impurity content of 9-(4-hydroxy-1-butyl)guanine into 200 g of dimethyl sulfoxide, heat to 60 ° C, keep warm until completely dissolved, and then add 5.5 g aluminum oxide, keep stirring for 1.0 h, filter while it is hot, collect the filtrate and lower the temperature to 15-20°C, add 450 ml of ethanol while stirring, and stir for 2 h to crystallize. Filter, wash the filter cake with a small amount of ethanol, and obtain Penciclovir 37.60g after the filter cake is dried under reduced pressure, wherein 9-(4-hydroxyl-1-butyl)guanine impurity is 0.06%.

Embodiment 2

[0026] Add 40 g of crude penciclovir with 1.40% impurity content of 9-(4-hydroxy-1-butyl) guanine into 320 g of dimethyl sulfoxide under stirring, heat to 60 ° C, keep warm until completely dissolved, and then add 22.4 g aluminum oxide, keep stirring for 1.0 h, filter while it is hot, collect the filtrate and lower the temperature to 15-20°C, add 450 ml of ethanol while stirring, and stir for 2 h to crystallize. Filter, wash the filter cake with a small amount of ethanol, and obtain Penciclovir 37.06g after the filter cake is dried under reduced pressure, wherein 9-(4-hydroxy-1-butyl)guanine impurity is 0.03%.

Embodiment 3

[0028] Under stirring, add 40 g of crude penciclovir with 2.10% impurity content of 9-(4-hydroxy-1-butyl)guanine into 200 g of dimethyl sulfoxide, heat to 60 ° C, keep warm until completely dissolved, and then add 27.0 g aluminum oxide, keep stirring for 0.5h, filter while it is hot, collect the filtrate and lower the temperature to 15-20°C, add 450ml of ethanol while stirring, stir and crystallize for 2h. Filter, wash the filter cake with a small amount of ethanol, and obtain Penciclovir 36.52g after the filter cake is dried under reduced pressure, wherein 9-(4-hydroxyl-1-butyl)guanine impurity is 0.07%.

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Abstract

The invention provides a purification method of penciclovir. The purification process comprises the following steps of heating and dissolving a crude penciclovir product with dimethyl sulfoxide, then adding aluminum oxide, stirring, filtering, adding a low-basic alcohol solvent to the filtrate, crystallizing, filtering and drying to obtain penciclovir. By virtue of the purification process disclosed by the invention, a penciclovir finished product of which the purity reaches above 99.9% and in which the content of 9-(4-hydroxy-1-butyl) guanine as an impurity is less than 0.10% can be obtained; the purification method has the advantages of simple operation, strong repeatability, no pollution, low cost and relatively high yield and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of compound preparation, in particular to a method for refining penciclovir. technical background [0002] Penciclovir is a purine derivative with antiviral activity. It belongs to nucleoside antiviral drugs. drug. The chemical name of penciclovir is 9-[4-hydroxyl-3-(hydroxymethyl)-butyl]-guanine, and its structural formula is as follows: [0003] [0004] In the synthesis of penciclovir, 2-amino-6-chloropurine is generally used as a raw material to couple with an alkyl halide under alkaline conditions, and then decarboxylate under alkaline conditions. During the decarboxylation reaction, a by-product that removes two molecules of carboxylic acid will be produced. After the subsequent reduction reaction, 9-(4-hydroxy-1-butyl)guanine impurity will be generated. Its structural formula is as follows. How to reduce penciclo The content of 9-(4-hydroxy-1-butyl)guanine impurity in Weiwei is rarely reported at present....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D473/18
CPCC07D473/18
Inventor 张颖刘鹏刘真豪马延国朱玉正高国锐刘元鑫王学斌李洪爽郑良文
Owner JINAN KANGHE MEDICAL TECH
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