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Method for refining Valsartan containing more than 10% of isomer

A purification method and isomer technology, applied in the field of medicine and chemical industry, can solve problems such as cost increase, no reported purification method, etc., and achieve the effect of reducing D-type isomer and high yield

Active Publication Date: 2010-07-07
ZHEJIANG HUAHAI PHARMACEUTICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If the D-type isomer is higher than 10% (HPLC detection peak area method), it is necessary to adopt ethyl acetate to refine repeatedly, and the refinement repeatedly will inevitably cause the improvement of cost, and existing literature does not report better refining method

Method used

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  • Method for refining Valsartan containing more than 10% of isomer

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 20.0g of valsartan containing 10.2% of the D-isomer (HPLC detection peak area method) and 60ml of butanone into a 100ml three-necked flask, heat to 40°C and stir to dissolve, then cool to -15°C and stir to crystallize, and precipitate Stirring was continued for about 5 hours, suction filtered, natural drying in a fume hood, and then vacuum drying at 30° C. to obtain 7.9 g of solid with a yield of 39%. The D-isomer was detected by HPLC as 0.28%.

Embodiment 2

[0018] Add 20.0g of valsartan containing 12.9% of the D-isomer (HPLC detection peak area method) and 100ml of butanone into a 250ml three-necked flask, heat to 40°C and stir to dissolve, then cool to -15°C and stir to crystallize, and precipitate Stirring was continued for about 5 hours, suction filtered, natural drying in a fume hood, and then vacuum drying at 30° C. to obtain 3.2 g of solid with a yield of 16%. The D-isomer detected by HPLC was 1.42%.

Embodiment 3

[0020] Add 25.0g of valsartan containing 12.9% of D-isomer (HPLC detection peak area method) and 125ml of butanone in a 500ml three-necked flask, heat to 40°C and stir to dissolve, then add 140ml of isopropyl ether, and cool to -15 Stir and crystallize at ℃, continue to stir for about 5 hours, filter with suction, and dry in vacuo at 35°C to obtain 12.7 g of solid with a yield of 50.8%. The D-isomer detected by HPLC is 3.8%.

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Abstract

The invention discloses a method for refining Valsartan containing higher isomer impurity, namely Valsartan containing more than 10% (HPLC detection peak area method) of N isomer is refined by adopting butanone or the mixture solvent of butanone and esters and ethers, the N isomer can be remarkably reduced to about 1.0%, and the yield can be as high as more than 50%.

Description

technical field [0001] The invention relates to a method for refining valsartan containing higher isomers (more than 10%), and belongs to the field of medicine and chemical industry. Background technique [0002] Valsartan (valsartan), chemical name N-(1-oxopentyl) N-[4-[2-(1H-tetrazol-5 base) phenyl] benzyl]-L-valine, is the following Another new type of antihypertensive drug after calcium ion channel blockers and angiotensin converting enzyme inhibitors (ACEI), it is an angiotensin II (angiotensin II) AT receptor antagonist, avoiding calcium antagonists and ACEI It has the advantages of significant curative effect and good tolerance. [0003] During the synthesis of valsartan, due to the influence of reaction conditions, some products will racemize, thereby converting from L-form to D-form isomer. If the D-type isomer is higher than 10% (HPLC detection peak area method), it needs to be refined repeatedly with ethyl acetate, which will inevitably cause cost increase, and ...

Claims

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Application Information

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IPC IPC(8): C07D257/04A61P9/12
Inventor 黄想亮陈伟万晓明
Owner ZHEJIANG HUAHAI PHARMACEUTICAL CO LTD
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