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A kind of refining method of penciclovir

A refining method, the technology of penciclovir, which is applied in the field of compound preparation, can solve problems such as inability to guarantee, and achieve the effects of low cost, high product purity and high yield

Active Publication Date: 2016-01-13
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, and 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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  • A kind of refining method of penciclovir
  • A kind of refining method of penciclovir
  • A kind of refining method of penciclovir

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 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 dry the filter cake under reduced pressure to obtain 37.06 g of penciclovir, wherein the impurity of 9-(4-hydroxy-1-butyl)guanine is 0.03%.

Embodiment 2

[0026] 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 dry the filter cake under reduced pressure to obtain 36.52 g of penciclovir, wherein the impurity of 9-(4-hydroxy-1-butyl)guanine is 0.07%.

Embodiment 3

[0028] Under stirring, add 40 g of crude penciclovir with 0.41% impurity content of 9-(4-hydroxy-1-butyl)guanine into 160 g of dimethyl sulfoxide, heat to 80 ° 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 360 ml of isopropanol while stirring, and stir for 2 h to crystallize. Filter, wash the filter cake with a small amount of isopropanol, and dry the filter cake under reduced pressure to obtain 38.60 g of penciclovir, wherein the impurity of 9-(4-hydroxy-1-butyl)guanine is 0.07%.

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Abstract

The invention provides a method for refining penciclovir. The refining process specifically includes the following steps: heating and dissolving the crude product of penciclovir with dimethyl sulfoxide, then adding aluminum oxide to stir and filter, and adding low alcohol to the filtrate The solvent was crystallized, filtered, and dried to obtain penciclovir. Adopting the present invention can obtain the penciclovir finished product with a purity of more than 99.9% and a 9-(4-hydroxy-1-butyl)guanine impurity content of less than 0.10%. Pollution, low cost and high yield are 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 Patents(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