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Candesartan cilexetil compound and novel preparation method thereof

A technology for candesartan medoxomil and a compound is applied in the refining field of candesartan medoxomil, and can solve the problems of unsatisfactory drug purity, low total yield, reduced content of active pharmaceutical ingredients, and the like

Inactive Publication Date: 2011-05-25
HAINAN MEILAN SMITH KLINE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method total yield is low, and is not suitable for the needs of industrial production
[0007] In addition, when candesartan cilexetil is stored improperly or for too long, the content of the active ingredients of the drug will decrease, the color will increase, and the content of related substances will increase.
In some cases, the purity of the drug did not meet the requirements due to improper control of the manufacturing process

Method used

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  • Candesartan cilexetil compound and novel preparation method thereof
  • Candesartan cilexetil compound and novel preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Dissolve 100 g of candesartan cilexetil crude product with a purity of 97.3% in 1000 ml of acetonitrile, add 2 g of activated carbon, insulate at 50° C. and stir for 20 min, filter for decarburization, and collect the filtrate;

[0034] (2) Cool the above filtrate to room temperature, slowly add purified water, stir to produce a precipitate, and collect 95.1 g of the precipitate by filtration;

[0035] (3) Dissolve the above precipitate with 200ml of 1:1 petroleum ether (30-60°C) / ethyl acetate, add 200g of pretreated Sepabeads SP850 macroporous adsorption resin, and mix well to obtain the adsorbed candesartan cilexetil The resin is then added to the top of the Sepabeads SP850 type macroporous adsorption resin column, washed with purified water of 1 to 2 column volumes to clarification, then eluted with 30% ethanol eluent, and the eluted candesartan cilexetil is collected. The ethanol fraction was concentrated under reduced pressure and dried to obtain 92.5 g of refi...

Embodiment 2

[0037] (1) Dissolve 100 g of candesartan cilexetil crude product with a purity of 97.3% in 500 ml of acetone, add 1 g of activated carbon, stir at 50° C. for 10 min, filter for decarburization, and collect the filtrate;

[0038] (2) Cool the above-mentioned filtrate to room temperature, slowly add purified water, stir to produce a precipitate, and collect 94.8 g of the precipitate by filtration;

[0039] (3) Dissolve the above precipitate with 200ml of 1:1 petroleum ether (30-60°C) / ethyl acetate, add 200g of pretreated Sepabeads SP825901 type macroporous adsorption resin, and mix well to obtain the adsorbed candesartan cilexetil The resin is then added to the top of the Sepabeads SP825 type macroporous adsorption resin column, washed with purified water of 1 to 2 column volumes to clarification, then eluted with 30% ethanol eluent, and the eluted candesartan cilexetil is collected. The ethanol fraction was concentrated under reduced pressure and dried to obtain 90.1 g of refin...

Embodiment 3

[0041] (1) Dissolving 100 g of crude candesartan cilexetil with a purity of 97.3% in 2000 ml of methanol, adding 6 g of activated carbon, stirring at 50° C. for 30 min, filtering for decarburization, and collecting the filtrate;

[0042] (2) Cool the above-mentioned filtrate to room temperature, slowly add purified water, stir to produce a precipitate, and collect 94.4 g of the precipitate by filtration;

[0043] (3) Dissolving the above-mentioned precipitation with 200ml of 1:1 petroleum ether (30~60°C) / ethyl acetate, adding 200g of pretreated HPD300 type macroporous adsorption resin, mixing thoroughly to obtain the product of adsorbing candesartan cilexetil The resin is then added to the top of the HPD300 macroporous adsorption resin column, washed with 1 to 2 column volumes of purified water until clarified, then eluted with 30% ethanol eluent, and the ethanol part eluted by candesartan cilexetil is collected , concentrated under reduced pressure, and dried to obtain 88.4 g...

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Abstract

The invention provides a candesartan cilexetil compound and a novel preparation method thereof. Through absorption of active carbon, crystallization and adsorptive separation of macroporous absorption resin, the purpose of refined purification is achieved, and finally, the high-purity candesartan cilexeti is obtained, thereby greatly improving the purity and content of the candesartan cilexeti, improving the product quality of the preparation, reducing toxic and side effects and guaranteeing the clinical pharmacy safety of the candesartan cilexeti in preparing anti-hypertension medicaments. The novel preparation method has the advantages of simple process, low cost and high yield, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for refining candesartan cilexetil, through which a high-purity candesartan cilexetil product can be obtained, and belongs to the technical field of medicine. Background technique [0002] Candesartan cilexetil (Candesartan cilexetil), alias: candesartan cilexetil, candesartan cilexetil, suitable for the treatment of hypertension, jointly developed by Takeda Corporation of Japan and Astra Corporation of Sweden, First launched in Sweden in November 1997. Candesartan cilexetil is white or off-white crystalline powder, its chemical name is: (±)-1-(cyclohexyloxycarbonyloxy)ethyl-[2-ethoxy-1-[[2′- (1H-tetrazolyl-5)biphenyl-4]methyl]-1H-benzimidazole-7]carboxylate, molecular formula: C 33 h 34 N 6 o 6 , molecular weight: 610.67, structural formula: [0003] [0004] Candesartan cilexetil is rapidly hydrolyzed in vivo to the active metabolite candesartan. Candesartan is an angiotensin II AT1 receptor antagonist, whi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D403/10A61P9/12
Inventor 杨明贵
Owner HAINAN MEILAN SMITH KLINE PHARMA
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