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Process for refining olmesartan medoxomil by adopting mixed solution of acetone and water

A technology of olmesartan medoxomil and mixed solution, applied in the field of medicinal chemistry, can solve the problems of high solvent residue and low acetone solvent residue, and achieve the effects of low acetone residue, stable and uniform crystallization, and good refining effect.

Active Publication Date: 2012-07-11
ZHEJIANG HUAHAI PHARMACEUTICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem solved by the present invention is to provide a refining process using acetone / water to refine olmesartan medoxomil, which not only has good refining effect and high yield, but also has very low residue of acetone solvent, about 1000ppm, and solves the problem of solvent residue in the existing refining technology. too high problem

Method used

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  • Process for refining olmesartan medoxomil by adopting mixed solution of acetone and water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 25.0g olmesartan medoxomil (containing 1.2% olmesartan acid impurity content) and 375ml acetone into a 1L three-necked flask, heat and mechanically stir and reflux to dissolve. Take another 1L three-necked flask and add 375ml purified water, stir and heat to 45~50℃. Add the acetone / water solution of Olmesartan medoxomil before, and keep the temperature for 1 hour after the addition, stir for 3 hours under cooling in an ice-water bath, filter to dryness, and vacuum dry at 45-50℃ to obtain 23.8g of white solid product omesar The yield is 94.0%, the purity is 99.5%, olmesartan acid impurity is 0.12%, other single impurities are less than 0.1%, and acetone remains 710ppm.

Embodiment 2

[0018] Add 15g olmesartan medoxomil (containing 0.8% olmesartan acid content) and 225ml acetone to a 500ml glass bottle, mechanically stir to reflux and dissolve it, cool slightly, and pour it into a 1L glass bottle containing 225ml 40-45℃ water under stirring. Keep the temperature and stir for 1.5 hours, then cool to 15-20°C and stir for 3.5 hours, filter to dryness, and vacuum dry at 50°C for 16 hours to obtain 13.8 g of olmesartan medoxomil with 92.0% yield and 99.8% purity. Olmesartan acid Impurities are 0.05%, other single impurities are less than 0.1%, and acetone remains 1327ppm.

Embodiment 3

[0020] Add 25.0g olmesartan medoxomil (containing 0.8% olmesartan acid), 250ml acetone and 12.5ml purified water into a 1L three-necked flask, heat and mechanically stir to reflux to dissolve, stop heating and stirring. Add another 1L three-necked flask to 237.5ml purified water, and heat to 45-50℃ with mechanical stirring. Add olmesartan medoxomil acetone / aqueous solution, after the addition, keep stirring at this temperature for 1 hour, stir at room temperature for 2 hours, stir under ice-water bath cooling for 2 hours, filter and dry under vacuum at 45-50℃ to obtain 23.8g of white solid The product olmesartan medoxomil has a yield of 95.2%, purity of 99.8%, olmesartan acid impurity 0.02%, other single impurities are less than 0.1%, and acetone residue is 877 ppm.

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Abstract

The invention discloses a process for refining olmesartan medoxomil by adopting a mixed solution of acetone and water. The process comprises the steps that the olmesartan medoxomil is dissolved in the acetone or the mixed solution of the acetone and the water; then an obtained olmesartan medoxomil solution is added to hot water to be stirred and crystallized; and after the olmesartan medoxomil solution is filtered and dried, the olmesartan medoxomil is obtained. The process has the characteristics of good refining effect and high yield; and the acetone residual amount is small and can be controlled at about 1,000 ppm.

Description

Technical field [0001] The invention relates to a refining method of olmesartan medoxomil and belongs to the field of medicinal chemistry. Background technique [0002] Olmesartan medoxomil, English name is Olmesartan Medoxomil, chemical name: 4-(1-hydroxy-1-methylethyl)-2-propyl-1-{4-[2-(tetrazol-5-yl) Phenyl]phenyl)methylimidazole-5-carboxylic acid-(5-methyl-2-oxo-1,3-dioxol-4-yl)methyl ester, developed by Sankyo Company in Japan An orally effective non-peptide angiotensin II receptor antagonist. The drug was approved by the U.S. FDA in May 2002 under the trade name Banicar. Its outstanding advantage is that it has a long half-life, and it can be taken once a day to effectively control blood pressure in a day, so it is more convenient to take. At the same time, compared with other angiotensin II receptor antagonist drugs, olmesartan medoxomil has a small dose, quick onset, convenient administration, stronger and more durable antihypertensive effect, and a low incidence of ad...

Claims

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Application Information

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IPC IPC(8): C07D405/14
Inventor 黄想亮华媛媛张立武永德
Owner ZHEJIANG HUAHAI PHARMACEUTICAL CO LTD
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