Hydrolysable impurity compound of valsartan and preparation method, detection method and use thereof

A detection method and compound technology, applied in the field of medicine, can solve the problems of undisclosed impurity preparation methods and structural confirmation data, undisclosed application of hydrolyzed impurities, etc., to achieve good control and improve quality standards

Inactive Publication Date: 2014-10-01
NANJING CHIA TAI TIANQING PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The literature on valsartan is quite rich, mainly focusing on the synthesis route and crystal form. Regarding the impurity control of valsartan, Chinese patent CN102670485B discloses the preparation method of the solid composition of valsartan, and the hydrolyzed impurity H

Method used

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  • Hydrolysable impurity compound of valsartan and preparation method, detection method and use thereof
  • Hydrolysable impurity compound of valsartan and preparation method, detection method and use thereof
  • Hydrolysable impurity compound of valsartan and preparation method, detection method and use thereof

Examples

Experimental program
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Example Embodiment

[0039] Embodiment 1 Preparation of valsartan hydrolysis impurity compound

[0040] (1) Get 30g of valsartan, dissolve it in 200ml of acetonitrile, add 200ml of 6mol / L hydrochloric acid, heat and reflux for 4 hours, stir and drop to room temperature, then add 50% NaOH aqueous solution to adjust pH to neutral, separate phases, Add NaCl to the obtained aqueous phase to become a saturated solution, filter, extract the obtained saturated aqueous solution with n-butanol, take the organic phase, and evaporate to dryness to obtain a white solid;

[0041] (2) Dry the white solid in a vacuum drying oven, then beat with 10 times the weight of water at room temperature for 2 hours, and filter with suction to obtain the pure product. Through DEPT spectrum, COZY spectrum, HMBC, 1 H-NMR spectrum, 13 The structure was confirmed by C-NMR spectrum, and the analyzed data are shown in Table 1.

Example Embodiment

[0042] Embodiment 2 Preparation of valsartan hydrolysis impurity compound

[0043] (1) Get 30g of valsartan, dissolve it in 200ml of acetonitrile, add 300ml of 4mol / L hydrochloric acid, heat and reflux for 5 hours, stir and drop to room temperature, then add 60% NaOH aqueous solution to adjust pH to neutral, separate phases, Add NaCl to the obtained aqueous phase to become a saturated solution, filter, extract the obtained saturated aqueous solution with n-butanol, take the organic phase, and evaporate to dryness to obtain a white solid;

[0044] (2) Dry the white solid in a vacuum drying oven, then beat with 8 times the weight of water at room temperature for 3 hours, and filter with suction to obtain the pure product. Through DEPT spectrum, COZY spectrum, HMBC, 1 H-NMR spectrum, 13 The structure was confirmed by C-NMR spectrum, and the analyzed data are shown in Table 1.

Example Embodiment

[0045] Embodiment 3 Preparation of valsartan hydrolysis impurity compound

[0046](1) Get 30g of valsartan, dissolve it in 200ml of acetonitrile, add 140ml of 9mol / L hydrochloric acid, heat and reflux for 3 hours, stir and drop to room temperature, then add 40% NaOH aqueous solution to adjust pH to neutral, separate phases, Add NaCl to the obtained aqueous phase to form a saturated solution, filter, extract the obtained saturated aqueous solution with n-butanol, take the organic phase, and evaporate to dryness to obtain a white solid;

[0047] (2) Dry the white solid in a vacuum drying oven, then beat with 12 times the weight of water at room temperature for 1 hour, and filter to obtain the pure product. Through DEPT spectrum, COZY spectrum, HMBC, 1 H-NMR spectrum, 13 The structure was confirmed by C-NMR spectrum, and the analyzed data are shown in Table 1.

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Abstract

The invention discloses a hydrolysable impurity compound of valsartan, and discloses a preparation method and a detection method of the hydrolysable impurity compound, and use of the hydrolysable impurity compound for serving as an impurity reference substance for determination of valsartan related substances. Through preparation and structural confirmation of the compound, the reference substance is provided for analysis of the valsartan related substances, so as to improve the quality standard of valsartan, and provide important guiding significance for safe medication of valsartan.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a hydrolyzed impurity compound of valsartan, a preparation method, a detection method and application thereof. Background technique [0002] Valsartan (valsartan), chemical name: N-(1-oxopentyl)-N-[4-[2-(1H-tetrazol-5-yl)phenyl]benzyl]-L-valine , whose chemical formula is shown in formula Ⅱ, is an angiotensin receptor antagonist with a brand-new antihypertensive mechanism, stable antihypertensive, strong curative effect, long action time, and good tolerance of patients. Brain and kidney have a better protective effect. Patients with hypertension such as myocardial infarction, heart failure, proteinuria, and diabetes can be used as a conventional drug, and can also be used in combination with diuretics (such as hydrochlorothiazide). [0003] [0004] The literature on valsartan is quite rich, mainly focusing on the synthesis route and crystal form. Regarding the impurity contro...

Claims

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Application Information

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IPC IPC(8): C07D257/04G01N30/02
CPCC07D257/04G01N30/02
Inventor 钱修文吴舰朱谧柴雨柱杨治旻
Owner NANJING CHIA TAI TIANQING PHARMA
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