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Method for preparing vinpocetine

A technology of vinpocetine and vincamine, which is applied in the field of compound preparation, can solve the problems of three wastes treatment and adverse effects of solvent residues, unsuitable for large-scale industrial production, and short routes, etc., and achieves good reproducible results, easy handling, and less residues Effect

Active Publication Date: 2017-05-10
HENAN RUNHONG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Some need to use benzene or chlorobenzene in the dehydration process, and some need to use concentrated sulfuric acid, which will have adverse effects on the treatment of three wastes and solvent residues, so they are not suitable for large-scale industrial production
There is also a synthetic method using vincamine (the hydrolyzate of vincamine) as the starting material, but usually concentrated sulfuric acid, organic sulfonic acid, diaminopyridine, etc. are used, which easily cause environmental pollution; taking vinblastine as the starting material Among the synthetic methods, there is a method of using sulfonic acid type cation or styrene type anion exchange resin for esterification, dehydration and esterification to obtain the target product. This method produces relatively few wastes and has a short route, but it also uses concentrated sulfuric acid

Method used

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  • Method for preparing vinpocetine
  • Method for preparing vinpocetine
  • Method for preparing vinpocetine

Examples

Experimental program
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Effect test

Embodiment 1

[0098] This implementation takes vincamine as raw material, first prepares apovincamine, and then prepares vinpocetine with apovincamine as raw material.

[0099] The method that present embodiment prepares Vinpocetine comprises the steps:

[0100] 1) preparation of apovincamine

[0101] Put 15mL of NMP and 5g of vincamine into a 50mL dry and clean single-necked flask, stir for 5-10 minutes to obtain a uniform mixture, put an external ice-water bath to cool down to 0-5°C, add 1.62mL of thionyl chloride dropwise, and control the internal temperature. When the temperature exceeds 20°C, the dropwise addition is completed in half an hour. The ice bath was removed, and the temperature was raised to normal temperature (RT, 20-25° C.) in about 30 minutes, and the reaction was stirred for 30 minutes. The reaction was monitored by HPLC, and the reaction was terminated when the remaining amount of raw material vincamine was less than 1%. Then lower the temperature to 0-5°C, add 10mL ...

Embodiment 2

[0108] The purity of vincamine in this embodiment is not less than 99.3%.

[0109] This implementation uses vincamine as a raw material, firstly prepares apovincamine, and then prepares vinpocetine by using apovincamine as a raw material.

[0110] The method for preparing vinpocetine in the present embodiment comprises the following steps:

[0111] 1) Preparation of apovincamine

[0112] Put 690 mL of NMP and 230 g of vincamine in a 2000 mL dry and clean single-neck flask, stir for 5-10 minutes to obtain a uniform mixture, cool down to 0-5 ℃ in an external ice-water bath, add 74.8 mL of thionyl chloride dropwise, and control the internal temperature Above 20°C, the dripping is completed in about 1 hour. Remove the ice bath, stir and heat up to normal temperature (RT, 20-25 ℃) for about half an hour, monitor the residual amount of vincamine in the reaction with HPLC, end the reaction when the residual is less than 1%, then cool down to 0-5 ℃, add dropwise Purified water 460m...

Embodiment 3

[0120] The purity of vincamine in this embodiment is not less than 99.3%.

[0121] This implementation uses vincamine as a raw material, firstly prepares apovincamine, and then prepares vinpocetine by using apovincamine as a raw material.

[0122] The method for preparing vinpocetine in the present embodiment comprises the following steps:

[0123] 1. Preparation of apovincamine

[0124] Put 690 mL of NMP and 230 g of vincamine in a 2000 mL dry and clean single-neck flask, stir for 5-10 minutes to obtain a uniform mixture, cool down to 0-5 ℃ in an external ice-water bath, add 74.8 mL of thionyl chloride dropwise, and control the internal temperature Above 20°C, the dripping is completed in about 1 hour. Remove the ice bath, stir and heat up to normal temperature (RT, 20-25 ℃) for about half an hour, monitor the residual amount of vincamine in the reaction with HPLC, end the reaction when the residual is less than 1%, then cool down to 0-5 ℃, add dropwise Purified water 460m...

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Abstract

The invention relates to a method for preparing a compound, specifically to a method for preparing vinpocetine. The method comprises the following steps: 1) preparation of a vinpocetine crude product, including, mixing an apovincamine ethanol solution and a sodium ethoxide ethanol solution for a reflux reaction, removing the solvent, adding ethanol, carrying out a reflux reaction of the sodium ethoxide ethanol solution, when the residual content of apovincamine is less than 0.3% of the added apovincamine raw material, performing hot filtration, removing a part of solvent of the filtered liquid, and performing cooling crystallization, solid-liquid separation, washing and drying to obtain the vinpocetine crude product; and 2) refining of vinpocetine, including adding active carbon, performing hot filtration, and performing recrystallization with ethanol for refining to obtain vinpocetine. The method is short and simple in process. The prepared vinpocetine is high in yield and purity, meets the standard of the European Pharmacopoeia (EP) 6.0, and is easy for industrial production.

Description

technical field [0001] The invention relates to a method for preparing compounds, in particular to a method for preparing vinpocetine. Background technique [0002] Vinpocetine (Vinpocetine, trade name Vinpocetine, Kang Wei Nao), also known as Kalan Calan), is from Vincamajor, Vincaminor, a common evergreen plant similar to vines, distributed in central and southern Europe, etc. It has been used as a medicinal plant for nearly 2,000 years, and it is used by folks to cheer up, restore fatigue, especially similar symptoms related to aging, and is also used as an astringent, etc.), a natural indole alkaloid drug. [0003] The structural formula of Vinpocetine is as follows: [0004] [0005] Vinpocetine can selectively improve the blood circulation of the brain, promote the energy metabolism of the brain, regulate the function of the neurotransmitter system, and protect the brain from ischemic and hypoxic damage in many ways. Symptoms associated with aging and have partic...

Claims

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Application Information

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IPC IPC(8): C07D461/00
CPCC07D461/00
Inventor 韩静石勇志郭强高志亮
Owner HENAN RUNHONG PHARMA
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