Preparation process of high-purity oxymatrine

A technology of oxymatrine and preparation process, applied in the direction of organic chemistry and the like, can solve the problems of lack of practicability, the purity cannot reach more than 99%, etc., and achieve the effects of low cost, high product purity and high quality

Inactive Publication Date: 2012-08-01
NINGXIA BAUHINIA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Oxymatrine has high medicinal value, and its preparation method is not much reported in the patent literature, and the purity of the prepared oxymatrine can only reach 98%, such as CN1111533C, the publication date is June 18, 2003 , pointed out that the purity of oxymatrine prepared in reality could not reach more than 99%, so it was not practical, and pointed out that there was no preparation process at that time that could produce oxymatrine with a purity of more than 99%.

Method used

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  • Preparation process of high-purity oxymatrine

Examples

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Effect test

Embodiment 1

[0027] Add water to the oxidation tank and heat it up to 75°C, add 51g of analytically pure hydrogen peroxide, slowly add 100g of crude matrine in crystallized water, and react at 61°C for 13 hours, extract unreacted matrine with toluene until it reaches the reaction solution. Basically no matrine, concentrate under vacuum and decompression, recover water to dryness; add ethanol to dissolve, add aluminum oxide (Al 2 o 3 ) 30g for decolorization, suction filtration; vacuum concentration again, recovery of ethanol to dryness, adding acetone to melt, cooling and crystallization, centrifugation to obtain 101g of crude oxymatrine, the crude product of oxymatrine was dissolved in ethanol, and the ethanol solution was passed through The decolorizing agent is decolorized, the decolorized solution is suction-filtered, the ethanol is recovered, acetone is added to stir, cooling and crystallization is carried out, and 95 g of fine oxymatrine is obtained by centrifugation, and the content...

Embodiment 2

[0029] Add water to the oxidation tank and heat it to 75°C, add 51g of analytically pure hydrogen peroxide, slowly add 100g of crude matrine in crystallized water, and react at 59°C for 12 hours, extract the unreacted matrine with benzene until it is in the reaction solution There is basically no matrine, concentrated under reduced pressure in vacuum, and recovered water to dryness. Add ethanol to dissolve, add aluminum oxide (Al 2 o 3 ) 30g for decolorization, suction filtration; vacuum concentration again, recovery of ethanol to dryness, adding acetone to melt, cooling and crystallization, centrifugation to obtain 97g of crude oxymatrine, the crude oxymatrine was dissolved in ethanol, and the ethanol solution was passed through The decolorizing agent is decolorized, the decolorized solution is suction-filtered, the ethanol is recovered, acetone is added to stir, cooling and crystallization is carried out, and 92.8 g of fine oxymatrine is obtained by centrifugation, and the ...

Embodiment 3

[0031] Add water to the oxidation tank and heat it to 75°C, add 51g of analytically pure hydrogen peroxide, slowly add 100g of crude matrine in crystallized water, and react at 62°C for 12 hours, then extract the unreacted matrine with toluene until it reaches the reaction solution. There is basically no matrine, concentrated under reduced pressure in vacuum, and recovered water to dryness. Add ethanol to dissolve, add aluminum oxide (Al 2 o 3 ) 30g for decolorization, suction filtration; vacuum concentration again, recovery of ethanol to dryness, adding acetone for hot melting, cooling and crystallization, centrifugation to obtain 101g of crude oxymatrine, adding ethanol to dissolve the crude oxymatrine, and ethanol solution through The decolorizing agent is used for decolorizing, the decolorizing solution is suction-filtered, the ethanol is recovered, acetone is added to stir, cooling and crystallization is carried out, and 95.6 g of fine oxymatrine is obtained by centrifug...

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Abstract

The invention provides a preparation process of high-purity oxymatrine. The method comprises the following steps of: firstly, heating purified water in a water bath to a certain temperature; adding hydrogen peroxide and slowly adding oxymatrine to react at the certain temperature until the hydrogen peroxide is completely consumed; then, extracting residual less oxymatrine; decompressing and concentrating a reaction solution and adding an alcohols substance into the concentrated solution to be dissolved; adding a de-coloring agent for decoloring and filtering; continually decompressing and concentrating; adding an acetones substance to crystallize; and re-crystallizing to obtain the oxymatrine. The process method disclosed by the invention has the advantages of simplicity and practical applicability, low cost and high yield; and more importantly, the purity is high and the preparation process is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation process of high-purity oxymatrine. Background technique [0002] Traditional Chinese medicine Sophora flavescens, Sophora flavescens, and Sophora flavescens belong to leguminous plants. As the main source of oxymatrine, the three have the effects of clearing away heat and dampness, killing insects and diuresis. Among them, Sophora flavescens mainly contains alkaloids and flavonoids. Pharmacological experiments have proved that the total alkaloids have anti-arrhythmic and anti-cancer activities. Sophora flavescens contains a large amount of matrine, among which the highest content is matrine and oxymatrine, and there are other similar alkaloids, mainly sophocarpine, sophoramine, sophoridine, iso Matrine and other alkaloid components. [0003] Oxymatrine, also known as matrine, molecular formula C 15 h 24 N 2 o 2 ,White needle-like prism crystal or white crystalline powder, odorless, bitter taste. This strai...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/22
Inventor 不公告发明人
Owner NINGXIA BAUHINIA PHARMA
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