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Preparation method of high-purity vinpocetine

A vinpocetine and high-purity technology, which is applied in the field of high-purity vinpocetine preparation, can solve the problems of unsatisfactory impurity profiles in consistency evaluation, and achieve the effects of avoiding highly toxic reagents, simple production operation, and high purity

Active Publication Date: 2020-04-03
GUANGZHOU YIPINHONG PHARMA +4
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The production operation of the process of the present invention is simple and controllable; the obtained product has high purity and less impurities, and can solve the problem that the impurity spectrum of the consistency evaluation does not meet the requirements

Method used

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  • Preparation method of high-purity vinpocetine
  • Preparation method of high-purity vinpocetine
  • Preparation method of high-purity vinpocetine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] 1, the preparation of vincamine:

[0045] 1.1 Preparation of 15% (w / w) sodium hydroxide solution: Weigh 17.0kg of purified water and put it into a stainless steel bucket, then add 3.0kg of sodium hydroxide, stir well and let stand for later use.

[0046] 1.2 Add 3.0kg of tabonin, 0.3kg of activated carbon, and 27.0kg of tetrahydrofuran into a 50L double-layer glass reactor, and stir at room temperature for 2 hours for decolorization. Among them, the addition of activated carbon can adsorb toxic substances and prevent catalyst poisoning.

[0047] 1.3 Remove activated carbon by filtration, rinse with 1.5 kg of tetrahydrofuran (to clean residual active ingredients in activated carbon).

[0048] 1.4 Add 0.3kg of 10% palladium carbon to the filtrate and mix well, then transfer to a 50L magnetic drive reactor, N 2 Replaced three times, H 2 Replace three times (use nitrogen to drive off oxygen, prevent hydrogen and oxygen from mixing, causing danger. Another oxygen is not c...

Embodiment 2

[0090] On the basis of Example 1, in step 3.1: add 1.5kg of apovincamine, 12.0kg of absolute ethanol, 45.0g of sodium ethylate, and 3.0kg of dichloromethane into a 50L double-layer glass reactor, and heat up to 60-70°C React for 1 hour. The same detection method as in Example 1 was tested, and the purity was 99.90%.

Embodiment 3

[0092] On the basis of Example 1, in step 3.1: add 1.5kg of apovincamine, 12.0kg of absolute ethanol, 45.0g of sodium ethylate, and 3.0kg of dichloromethane into a 50L double-layer glass reactor, and heat up to 60-70°C React for 4 hours. The same detection method as in Example 1 was tested, and the purity was 99.92%.

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Abstract

The invention discloses a preparation method of high-purity vinpocetine. The preparation method comprises the following steps: S1, preparing vincamine, wherein tabersonine is dissolved, a hydrogenation reaction is performed under the catalysis of palladium and carbon to obtain vincadifformine, the vincadifformine is oxidized to obtain a vincadifformine nitric oxide, and an intermediate vincamine is obtained from the vincadifformine nitric oxide reaction liquid under the catalysis of an acid; S2, dewatering the vincamine by using toluene as a solvent and adding a dewatering agent to obtain apovincamine; and S3, on the basis of the step S2, carrying out a transesterification reaction by taking ethanol as a solvent, using dichloromethane as a cosolvent and using sodium ethoxide / sodium methoxide as a catalyst to obtain a vinpocetine crude product, and re-crystallizing with ethanol to obtain vinpocetine. The process provided by the invention has the advantages of simple production operation, avoidance of high-toxicity reagents, less impurity of the obtained product, high production efficiency, simple and convent operation and environmental friendliness, wherein the purity of the productis more than 99.9%, the quality of the product is higher than the quality of the product obtained by the original research factory, and the medicinal requirements are met.

Description

technical field [0001] The invention relates to the technical field of organic synthesis and is applied in the pharmaceutical industry, in particular to a preparation method of high-purity vinpocetine. Background technique [0002] Vinpocetine, also known as apovincine ethyl ester, is semi-synthesized from the monoindole alkaloid vincamine. As a cerebral vasodilator, vinpocetine can maintain or restore the physiological expansion of cerebral blood vessels, increase the normal cerebral blood flow in the ischemic area, improve the utilization rate of blood oxygen in the brain, and improve the metabolism of hypoxic brain tissue. It is widely used in the treatment and prevention of ischemic cerebrovascular diseases. [0003] Vinpocetine (Vinpocetine) was developed by the Jirui Pharmaceutical Company in Hungary and was launched in 1978. It is a conventional drug for treating cardiovascular and cerebrovascular diseases, and is known as one of the world's top ten longevity and an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D461/00
CPCC07D461/00
Inventor 李捍雄王小波王杰成
Owner GUANGZHOU YIPINHONG PHARMA
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