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Method for recovering valsartan racemate

A technology of valsartan racemate and recovery method, which is applied to the recovery field of valsartan racemate, can solve problems such as being unfavorable to environmental protection, waste resources and the like, and achieve environmental protection, good product quality and high yield. Effect

Active Publication Date: 2012-02-15
浙江新赛科药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This move is not only a waste of resources, but also not conducive to environmental protection, which deviates from the circular economy advocated by the country.

Method used

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  • Method for recovering valsartan racemate
  • Method for recovering valsartan racemate
  • Method for recovering valsartan racemate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1 Preparation of valsartan devaleryl product and n-valeric acid

[0033] Get 952g of ethyl acetate liquid of valsartan racemate and join in the reaction bottle of 2L, be heated up to 85 ℃ and steam ethyl acetate, when there is no distillate, obtain 582g (1.34mol) valsartan racemate, 463g of hydrochloric acid aqueous solution with a mass percentage concentration of 24% (including 3.04mol of hydrochloric acid) was added dropwise at heat preservation, and the solution was refluxed at 95° C. for 4 hours after dropping, cooled, and suction filtered. Recover the dry solvent from the filtrate under reduced pressure at 70°C to obtain product a: n-valeric acid, with a molar yield of 98%; add the filter cake to a 1000ml reaction flask, add 300ml of ice water, stir for about 30 minutes, and filter with suction. The filter cake was washed with ice water to weakly acidic pH=6.5, and dried to obtain the valsartan devaleryl product with a molar yield of 98%. The conversion ra...

Embodiment 2

[0045] Example 2 Preparation of valsartan devaleryl product and n-valeric acid

[0046] Get 952g of ethyl acetate liquid of valsartan racemate and join in the reaction bottle of 2L, be heated up to 85 ℃ and steam ethyl acetate, when there is no distillate, obtain 582g (1.34mol) valsartan racemate, 679g of hydrochloric acid aqueous solution with a mass percentage concentration of 36% (including 6.69 mol of hydrochloric acid) was added dropwise at heat preservation, and the solution was refluxed at 100°C for 4 hours after dropping, cooled, and suction filtered. Recover the dry solvent from the filtrate under reduced pressure at 70°C to obtain the product a: n-valeric acid, with a molar yield of 92%; add the filter cake to a 1000ml reaction flask, add 300ml of ice water, stir for about 30 minutes, and filter with suction. The filter cake was washed with ice water to weakly acidic pH=6.0, and dried to obtain valsartan devaleryl product with a molar yield of 92%. The conversion ra...

Embodiment 3

[0058] Example 3 Preparation of valsartan devaleryl product and n-valeric acid

[0059] Take 952g of ethyl acetate solution of valsartan racemate and add it to a 2L reaction flask, heat up to 85°C to distill the ethyl acetate, and when there is no distillate, 582g (1.34mol) of valsartan racemate is obtained 458 g (4.01 mol of hydrochloric acid) was added dropwise with a mass percent concentration of 32% hydrochloric acid solution at an insulated temperature, refluxed at 98° C. for 4 h after dropping, cooled, and suction filtered. Recover the dry solvent from the filtrate under reduced pressure at 70°C to obtain product a: n-valeric acid, with a molar yield of 94%; add the filter cake to a 1000ml reaction flask, add 300ml of ice water, stir for about 30 minutes, and filter with suction. The filter cake was washed with ice water to weakly acidic pH=6.8, and dried to obtain valsartan devaleryl product with a molar yield of 94%. The conversion rate was 98%.

[0060] Confirmation...

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Abstract

The invention discloses a method for recovering valsartan racemate, which comprises the following steps that: (1) pentanoic acid and valsartan depentanized acyl products are obtained through hydrolysis reaction of valsartan racemate in acid aqueous solution; and (2) in alcohol solvents, the valsartan depentanized acyl products take reduction reaction under the effect of reducing agents and catalysts to obtain valine and 4'-methyl phenylbenzene-2-hydroxyphenyl tetrazole. The method has the advantages that the steps are simple and convenient, the method is applicable to industrial production, and the 4'-methyl phenylbenzene-2- hydroxyphenyl tetrazole, the valine and the pentanoic acid can be recovered, wherein the 4'-methyl phenylbenzene-2-tetrazole is an important raw material for synthesizing losartan important intermediate N-(trityl)-5-(4'-bromine methyl phenylbenzene)-2-hydroxyphenyl) tetrazole.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, and in particular relates to a method for recovering a racemate of valsartan. Background technique [0002] Valsartan (chemical name: N-(1-pentanoyl)-N-[4-[2-(1H-tetrazol-5-yl)phenyl]benzyl]-L-valine) available It is suitable for various types of hypertension, and has a good protective effect on the heart, brain and kidney. Hypertensive patients such as myocardial infarction, heart failure, proteinuria, and diabetes can be used routinely, and can be used in combination with diuretics (such as hydrochlorothiazide). Valsartan molecular formula: C 24 h 29 N 5 o 3 , molecular weight: 435.52, CAS number: 137862-53-4, the structural formula is as follows: [0003] [0004] Valsartan is a chiral drug. At present, there are many manufacturers of valsartan, but the production process is to use the chiral raw material as the starting material to obtain valsartan through a series of reactions. Du...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D257/04C07C229/08C07C227/18C07C53/126C07C51/06
Inventor 杨和军胡宇宏吕士华宋光伟许永平郭洪巨
Owner 浙江新赛科药业有限公司
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