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Preparation method of vinpocetine

A technology of vinpocetine and vincristine, which is applied in the direction of organic chemistry, etc., can solve the problems that the product quality cannot meet the high-quality requirements of raw materials, harsh reaction conditions, and high toxicity of reagents, and can meet the requirements of quality, stable quality and operation. easy effect

Active Publication Date: 2013-09-11
BEIJING AOHE DRUG RES INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The preparation methods of vinpocetine reported in these literatures all have defects such as high reagent toxicity, harsh reaction conditions, complicated operation, and product quality that cannot meet the high-quality requirements of raw materials.

Method used

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  • Preparation method of vinpocetine
  • Preparation method of vinpocetine
  • Preparation method of vinpocetine

Examples

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Embodiment 1

[0035] Example 1 The preparation method of vinpocetine

[0036] The preparation method of present embodiment Vinpocetine, comprises the steps:

[0037] 1) Add 10 grams of concentrated sulfuric acid and 5 grams of vinblastine to 100 grams of absolute ethanol. After stirring and dissolving, slowly add 10 grams of thionyl chloride dropwise at 0-10°C, heat to 80°C, and react for 24 hour, the reaction solution was prepared;

[0038] 2) Concentrate the reaction solution under reduced pressure, dilute the concentrated residue with 50ml of water, adjust the pH to 7-8, and extract with dichloromethane (50ml×2);

[0039] 3) After the dichloromethane extract phases were combined, they were washed with 50 ml of saturated brine, dried over anhydrous magnesium sulfate, filtered, the filtrate was concentrated under reduced pressure at 40°C, and the concentrated residue was recrystallized with absolute ethanol to obtain 3.5 g of Vinpocetine .

[0040] The melting point of V...

Embodiment 2-13

[0041] Example 2-13 The preparation method of vinpocetine

[0042] The preparation method of Vinpocetine described in embodiment 2-13, comprises the steps:

[0043] 1) Add 10 grams of concentrated sulfuric acid, 5 grams of vinblastine and the sulfonic acid or sulfonate described in Table 1 to 100 grams of absolute ethanol, stir and dissolve, heat to the temperature conditions described in Table 1, and react 12 to 24 hour, the reaction solution was prepared;

[0044] 2) Concentrate the reaction solution under reduced pressure, dilute the concentrated residue with 50ml of water, adjust the pH to 7-8, and extract with dichloromethane (50ml×2);

[0045] 3) After the dichloromethane extracts were combined, they were washed with 50 ml of saturated brine, dried over anhydrous magnesium sulfate, filtered, and the filtrate was concentrated under reduced pressure at 40°C, and the concentrated residue was recrystallized with absolute ethanol to obtain Vinpocetine.

[004...

Embodiment 14-16

[0049] Examples 14-16 The preparation method of vinpocetine

[0050] The preparation method of Vinpocetine described in embodiment 14-16, comprises the steps:

[0051] 1) Add concentrated sulfuric acid, 5 grams of vinblastine and methanesulfonic acid into absolute ethanol (the amount of the aforementioned substances is as described in Table 2), stir and dissolve, heat to 80°C, and react for 24 hours to obtain a reaction solution ;

[0052] 2) Concentrate the reaction solution under reduced pressure, dilute the concentrated residue with 50ml of water, adjust the pH to 7-8, and extract with dichloromethane (50ml×2);

[0053] 3) After the dichloromethane extracts were combined, they were washed with 50 ml of saturated brine, dried over anhydrous magnesium sulfate, filtered, and the filtrate was concentrated under reduced pressure at 40°C, and the concentrated residue was recrystallized with absolute ethanol to obtain Vinpocetine.

[0054] The melting point, yiel...

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Abstract

The invention relates to a preparation method of vinpocetine. The preparation method comprises the following steps of: (1) in the presence of mixed acid, reacting apovincaminic acid with absolute ethyl alcohol in a heating condition to obtain a reaction solution; (2) condensing the reaction solution at reduced pressure, diluting the concentration residue using water, adjusting the pH (Potential of Hydrogen) to 8-9, carrying out extraction by using an organic phase, washing the organic phase by using a saturated saline solution, dewatering and drying the organic phase, and carrying out filtration, reduced-pressure concentration and recrystallization, and drying to obtain the vinpocetine. The preparation method provided by the invention has the characteristics of environment protection and the like and is simple and convenient to operate, and the prepared vinpocetine has the advantages of high purity, controllable impurity, low cost and the like.

Description

[0001] technical field [0002] The invention belongs to the field of drug synthesis, and in particular relates to a preparation method of vinpocetine. Background technique [0003] Vinpocetine (Vinpocetine, whose structure is shown in formula 1), also known as apovincine ethyl ester, is a structurally modified derivative of vincamine (structure shown in formula 2), developed by the Hungarian pharmaceutical company Cedeon Richter in 1978 listed. Clinical data confirm that Vinpocetine can selectively improve brain blood circulation, promote brain energy metabolism, regulate neurotransmitter system functions, and protect the brain from ischemia and hypoxia damage in many ways. It is used for cardiovascular and cerebrovascular diseases, ischemia Hypertensive encephalopathy, cerebral arteriosclerosis, cerebral ischemia, intermittent cerebral blood flow insufficiency, cerebral vasospasm, cerebral thrombosis, and brain diseases caused by aging, and the curative effect is remarkab...

Claims

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Application Information

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IPC IPC(8): C07D461/00
Inventor 程晓峰霍彩霞黄晓霞屈英薇张洋
Owner BEIJING AOHE DRUG RES INST
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