Method for synthesizing medication Entecavir of anti hepatitis B

A technology of entecavir and formula, applied in the synthesis field of anti-hepatitis B drugs, can solve the problems of low purity and high cost of entecavir, and achieve the effects of high product purity, low price and cost reduction

Active Publication Date: 2007-10-10
江西科睿药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The invention overcomes the defects of high cost and low purity of entecavir in the prior art, and provides a preparation method that can greatly reduce the cost and improve the purity of entecavir
[0006] The purpose of the present invention is to overcome the defects of high cost and low purity of entecavir in the prior art, and provide a preparation method that can greatly reduce the cost and improve the purity of entecavir

Method used

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  • Method for synthesizing medication Entecavir of anti hepatitis B
  • Method for synthesizing medication Entecavir of anti hepatitis B
  • Method for synthesizing medication Entecavir of anti hepatitis B

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Preparation of Entecavir

[0042]

[0043] Each specific process in the above-mentioned reaction is respectively:

[0044] 1. Preparation of (1α, 4α, 5α)-7,7-dichloro-4-(diphenylmethylsilyl)-cyclo(3,2,0)-heptane-2-cyclo-6-one

[0045] a) Reaction equation

[0046]

[0047] b) Detailed operation process

[0048] 100g of dicyclopentadiene was added to a 250ml four-necked flask, N 2 Under protection, the temperature was heated to 180-190°C, and then the fraction at 40-42°C was slowly collected to obtain 65 g of cyclopentadiene monomer.

[0049] In a 500ml four-necked bottle equipped with mechanical stirring, add 300ml of THF and 20g of sodium metal, 2 65 g of cyclopentadiene monomer was added dropwise under protection, and then stirred and reacted at room temperature for 10 hours. After the reaction, the unreacted solid was filtered off and used directly for the next reaction.

[0050] In another 2L four-neck flask equipped with mechanical stirring, with a 500m...

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Abstract

This invention discloses a method for synthesizing entecavir as an anti-hepatitis B drug. The method is characterized by: diphenyl methylchlorosilane is utilized as a protective agent is step 1, and cyclohexyl methanol is utilized as an esterifying agent in step 4. The method has such advantages as low cost, high drug purity and high yield, and is suitable for industrialization.

Description

technical field [0001] The invention relates to a method for synthesizing anti-hepatitis B medicine, in particular, the invention relates to a method for preparing anti-hepatitis B medicine entecavir. Background technique [0002] Entecavir (Entecavir) is a cyclopentylguanine nucleoside analogue, which is a selective oral nucleoside drug against HBV. Foreign patents on synthesis mainly include: WO9809964 and WO2004052310. In the circuit reported in WO980996, column chromatography is required for the purification of reaction intermediates in basically every step, and the purification of the final product obtained is also very difficult and the yield is very low, so it is generally not used. The synthetic route of Bristol-Myers Squibb Company (i.e. WO2004052310) uses sodium cyclopentadiene as a raw material, and through a series of reactions, the final product is obtained. The synthetic route is shown in the figure below: [0003] [0004] Compared with WO9809964, this ro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D473/18A61K31/522A61P1/16A61P31/14
CPCY02P20/55
Inventor 姜维斌王万青胡雅芳
Owner 江西科睿药业有限公司
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