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Preparation method of high-purity nitrendipine bulk drug

A technology of high-purity nitrendipine and nitrendipine, which is applied in the field of preparation of high-purity nitrendipine raw materials, can solve the problems of impurity B and impurity C control, and the quality data of nitrendipine is not given, so as to avoid impurities B and Formation of Impurity C, High Yield, Effect of Guaranteed Yield

Pending Publication Date: 2022-03-08
天津太平洋化学制药有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0016] Patent CN109232390A reports a three-step method for synthesizing nitrendipine, which does not control impurities B and C, and does not give quality data of nitrendipine

Method used

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  • Preparation method of high-purity nitrendipine bulk drug
  • Preparation method of high-purity nitrendipine bulk drug
  • Preparation method of high-purity nitrendipine bulk drug

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Embodiment 1

[0057] Pump 90.0kg of ethyl acetoacetate and 5.0kg of 98% concentrated sulfuric acid into a 1000L kettle, add 100.0kg of m-nitrobenzaldehyde in batches, heat up during the feeding process, and stir the reaction at 20-25°C after the addition is complete 2 to 8 hours; the reaction system is gradually solidified, and after the completion of the reaction, the crude product 2-(3-nitrobenzylidene)ethyl acetoacetate is obtained; add 200kg of water to the reaction kettle for beating and dispersion, and after stirring for 20 minutes, discharge the material for centrifugation Shake off the filter, centrifuge the solid and beat it with 200kg of water to disperse it, centrifuge again, and dry the centrifuged solid at 40-45°C for 12 hours to obtain about 155.0kg of pure ethyl 2-(3-nitrobenzylidene)acetoacetate (content 98.74%, yield 89.10%);

[0058] Add 150.0kg of ethyl 2-(3-nitrobenzylidene)acetoacetate to 480.0kg of ethanol, then add 85.0kg of methyl 3-aminocrotonate, and then add 30.0k...

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Abstract

The invention provides a preparation method of a high-purity nitrendipine raw material medicine, which comprises the following steps: preparing a crude product 2-(3-nitrobenzylidene) ethyl acetoacetate at normal temperature by taking ethyl acetoacetate, 98% concentrated sulfuric acid and m-nitrobenzaldehyde as raw materials; then washing, centrifuging and drying to obtain a pure product 2-(3-nitrobenzylidene) ethyl acetoacetate; the preparation method comprises the following steps: adding ethyl 2-(3-nitrobenzylidene) acetoacetate into an organic solvent, then adding methyl 3-aminocrotonate and a moisture scavenger, carrying out heating reaction, after the reaction is finished, removing the moisture scavenger, cooling, stirring, centrifuging, and drying a solid to obtain nitrendipine. The purity of the nitrendipine bulk drug obtained by the preparation method of the high-purity nitrendipine bulk drug is 99.80% or above, and the impurity B and the impurity C are both less than 0.1%.

Description

technical field [0001] The invention belongs to the field of chemical pharmacy, and in particular relates to a preparation method of a high-purity nitrendipine crude drug. Background technique [0002] Nitrendipine (NTD) was first developed by Bayer AG of Germany and started production in the 1970s. Trade name: Bayotensin. Nitrendipine Tablets is a dihydropyridine calcium channel blocker, which can inhibit the transmembrane calcium ion influx in vascular smooth muscle and myocardium, and mainly acts on blood vessels, so it has strong vascular selectivity. Can cause coronary artery, renal arteriole and other blood vessels in the whole body to expand, and produce antihypertensive effect. Nitrendipine is widely used in the treatment of hypertension and coronary heart disease because of its rapid onset of action, long duration of drug effect, definite curative effect, and small side effects. The chemical structure of nitrendipine is as follows: [0003] [0004] In recent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/90
CPCC07D211/90
Inventor 宋香羿邴贵方于海燕杨荣珍余珍
Owner 天津太平洋化学制药有限公司
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