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Lappaconitine hydrobromide preparation method

A technology of alkali hydrobromide and labaconitine, which is applied in the direction of organic chemistry, can solve the problems of low product purity and high production cost, and achieve the effect of high product purity, low production cost and simple process

Inactive Publication Date: 2008-09-10
王小银
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of this invention is to provide a kind of preparation method of rabaconitine hydrobromide, to solve the problem that the product purity that existing technology makes is low, production cost is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Aconitum aconitum root is cleaned and crushed into coarse powder, soaked in sulfuric acid ethanol solution with an acid concentration of 0.3% (mass to volume content) in the total solution for 36 hours, percolation, and the percolation speed is 4ml / min·kg, Concentrate the percolation liquid under reduced pressure to liquid extract, cool, let it stand, filter, and adjust the filtrate to pH9.0 with 12% (weight percent) sodium hydroxide solution, extract with chloroform, and absorb the extract Filter the impurities, concentrate the extract until the solution precipitates crystals, dilute the solution containing the crystals with ethanol and let it stand for 20 hours, separate the crystals, and obtain the total alkaloids containing rabaaconitine. The total alkaloids were dissolved in 90% (volume percent) ethanol at a ratio of 1:10 (g:ml), filtered while hot, and the filtrate was allowed to stand for 32 hours to separate and crystallize to obtain the refined product of rabaco...

Embodiment 2

[0017] Aconitum aconitum root is cleaned and crushed into coarse powder, soaked in sulfuric acid ethanol solution with an acid concentration of 0.5% (mass to volume content) in the total solution for 48 hours, percolation, and the percolation speed is 4ml / min·kg, Concentrate the percolation liquid under reduced pressure to liquid extract, cool, let stand, filter, the filtrate is adjusted to PH9.2 with 12% (weight percent) sodium carbonate solution, extracted with chloroform, and the extract is absorbed by impurities After filtering, concentrate the extract until the solution precipitates crystals, dilute the solution containing the crystals with ethanol and let it stand for 16 hours, separate the crystals, and obtain the total alkaloids containing rabaconitine. Dissolve the total alkaloids in 85% (volume percent) ethanol at a ratio of 1:12 (g:ml), filter while hot, and let the filtrate stand for 60 hours to separate and crystallize to obtain the refined product of rabaconitine....

Embodiment 3

[0019] Aconitum aconitum root is cleaned and crushed into coarse powder, soaked in a sulfuric acid ethanol solution with an acid concentration of 0.8% (mass to volume content) in the total solution for 24 hours, percolation, and the percolation speed is 5ml / min·kg, Concentrate the percolation liquid under reduced pressure to liquid extract, cool, stand still, filter, adjust the filtrate to PH9.6 with concentrated ammonia water, extract with chloroform, filter the extract after absorbing impurities, concentrate the extract until the solution precipitates and crystallizes , Dilute the crystal-containing solution with ethanol and let it stand for 20 hours, separate the crystals, and obtain the total alkaloids containing rabaconitine. Dissolve the total alkaloids in 95% (volume percent) ethanol at a ratio of 1:15 (g:ml), filter while hot, and let the filtrate stand for 48 hours to separate and crystallize to obtain the refined product of rabaconitine. Dissolve this refined product...

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PUM

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Abstract

The invention discloses a preparing method of labaaconitine hydrobromide, which comprises the following steps: grinding sinomont root; extracting through acid alcohol penetrating method or acid water penetrating method; decompressing acid alcohol penetrating liquid to condense; obtaining fluid extract; cooling; stewing; filtering; adjusting pH value at 9-9.8 through alkalizer; extracting through trichloromethane; adding alkalizer in the acid water penetrating liquid to adjust pH value at 10-10.9; stewing; separating; leaving supernatant; dissolving sediment through trichloromethane; eluting through alcohol-trichloromethane; collecting extract or eluent; adsorbing impurity; filtering; condensing to obtain crystallized solution; diluting the solution through alcohol; stewing; separating; obtaining biological alkaline; recrystallizing through alcohol to obtain the refined product of labaaconitine; synthesizing the labaaconitine with hydrobromic acid to obtain the product.

Description

technical field [0001] The invention relates to a method for synthesizing rabaaconitine hydrobromide by extracting an active ingredient, rabaaconitine, from the root of the natural plant aconitum. Background technique [0002] Rabaaconitine hydrobromide (homoconitine hydrobromide) is an excellent non-addictive analgesic. It is widely used clinically to treat all kinds of pain, especially tumor pain. [0003] The existing method is to crush the root tubers of Aconitum aconitum, soak and percolate with ethanol to concentrate, extract the alkali with acid to free, extract and concentrate with chloroform, and then crystallize in ethanol, and the obtained total biological alkaloids are directly synthesized with hydrobromic acid. white. The product produced by this process has low purity. [0004] Existing methods include cutting or pulverizing the root tubers of Aconitum aconitum, and extracting them with ethanol reflux, ethanol dipping, and acid water percolation. The extrac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D221/22
Inventor 佘建文
Owner 王小银
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