Preparation technology of high-purity vinpocetine

A vinpocetine and preparation technology, which is applied in the field of preparation of high-purity vinpocetine, can solve the problems of limited product purity, serious environmental pollution, equipment corrosion, etc., achieve ideal yield and purity, simple operation process, reduce Effects of Environmental Pollution

Inactive Publication Date: 2013-02-20
孙新鹏
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above method uses a large amount of concentrated sulfuric acid, which seriously corrodes the equipment, and the three wastes are relatively large, causing serious environmental pollution. The post-treatment process of the product is cumbersome, and the purity of the product obtained is only 99.0%.

Method used

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  • Preparation technology of high-purity vinpocetine
  • Preparation technology of high-purity vinpocetine
  • Preparation technology of high-purity vinpocetine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] At room temperature, mix 3g of vincamine and 8ml of DMF and stir evenly, cool to 0-5 degrees, stir, and slowly add 0.96ml of SOCl dropwise 2 Into the reaction bottle (strictly control the reaction temperature not exceeding 30 degrees), react for 3 hours (room temperature 20-25 degrees), TLC and HPLC follow the reaction. After the raw materials disappear, cool to 0-5 degrees, add 250ml of ice water to quench, then cool to 0-5 degrees, add ammonia water (content 25%-28%) 83ml to adjust to PH=8 (strictly control the reaction temperature not to exceed 25 degree), a solid was precipitated, stirred within 10 degrees for half an hour, suction filtered, washed with a large amount of water, and washed with a small amount of ethanol to obtain 2.74 g of the intermediate Apovincamin. (Yield = 96%, HPLC: 99.8%)

Embodiment 2

[0039] At room temperature, mix and stir vincamine 3g and 7.2ml DMF evenly, cool to 0-5 degrees, keep stirring, slowly add 0.84ml SOCl dropwise 2 Into the reaction bottle (strictly control the reaction temperature not exceeding 30 degrees), react for 1 hour (room temperature 20-25 degrees), TLC and HPLC follow the reaction. After the raw materials disappear, cool to 0-5 degrees, add 15ml of ice water to quench (strictly control the reaction temperature not to exceed 25 degrees), then cool to 0-5 degrees, add ammonia water (content 25% to 28%) to adjust to PH = 8 (strictly control the reaction temperature not to exceed 25 degrees), precipitate solids, stir within 10 degrees for half an hour, filter with suction, wash with a large amount of water, and wash with a small amount of ethanol to obtain 2.74 g of the intermediate Apovincamin. (Yield = 96%, HPLC: 99.6%)

Embodiment 3

[0041] At room temperature, mix and stir 3g vincamine and 7.2ml DMF evenly, cool to 0-5 degrees, keep stirring, slowly add 0.66ml SOCl dropwise 2 Into the reaction bottle (strictly control the reaction temperature not exceeding 30 degrees), react for 1 hour (room temperature 20-25 degrees), TLC and HPLC follow the reaction. After the raw materials disappear, cool to 0-5 degrees, add 15ml of ice water to quench (strictly control the reaction temperature not to exceed 25 degrees), then cool to 0-5 degrees, add ammonia water (content 25%-28%) to adjust to PH = 8 (strictly control the reaction temperature not to exceed 25 degrees), precipitate solids, stir within 10 degrees for half an hour, filter with suction, wash with a large amount of water, and wash with a small amount of ethanol to obtain 2.74 g of the intermediate Apovincamin. (Yield = 96%, HPLC: 99.5%)

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Abstract

The invention relates to an optimized preparation technology of high-purity vinpocetine. According to the invention, vincamine is used as a raw material, a high-purity dehydrated methyl ester intermediate is obtained through a dehydration reaction, and then the vinpocetine is directly generated by an ester exchange reaction; or the dehydrated methyl ester intermediate is subjected to basic hydrolysis to generate corresponding acid, then thionyl chloride is dropwise added into the absolute ethyl alcohol solution of the acid, and the vinpocetine is generated by an esterification reaction. Through the invention, the production cost is obviously reduced, little environmental pollution is caused, the experimental operation is simple, the product is easy to separate and purify, and the product purity exceeds 99.8%.

Description

technical field [0001] The invention relates to an optimized preparation process of high-purity vinpocetine. Background technique [0002] Vinpocetine is a derivative of the indole alkaloid vincamine (I) extracted from Apocynaceae Vinca minor through structural modification. Vinpocetine has a variety of pharmacological effects beneficial to cardiovascular, cerebrovascular, blood circulation and other systems. It can promote the uptake and utilization of glucose and oxygen in the brain, increase ATP, reduce the production of lactic acid during ischemia and hypoxia; prevent brain cell excitation Toxic death (excessive receptor excitation caused by excitatory amino acids); reduce brain hypoxic damage, protect neurons; prevent ischemic damage to the brain, liver, muscle tissue and other parts; reduce aging brain dysfunction; promote Vasodilation, improve blood circulation; improve the deformability of red blood cells; increase cardiac output and nutrient blood flow to prepare o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D461/00
Inventor 刘苏友马大友秦粼陈正收
Owner 孙新鹏
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