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Method for preparing tanshinone IIA sodium sulfonate by using tanshinone crude extract

A technology of tanshinone and sodium sulfonate, applied in the fields of steroids, organic chemistry, etc.

Inactive Publication Date: 2014-05-07
华药控股有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no report on the method of directly using the crude extract of tanshinone as a raw material to prepare sodium tanshinone IIA sulfonate in the prior art

Method used

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  • Method for preparing tanshinone IIA sodium sulfonate by using tanshinone crude extract

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Add 200 g of tanshinone crude extract (tanshinone IIA content is about 60%) to 800 ml of acetonitrile solvent, then add 80 g of sulfur trioxide-pyridine complex with stirring. The reaction solution was heated to 65 degrees Celsius and stirred, and cooled to room temperature after the reaction was completed. The reaction solution was filtered, and the filter cake was washed 3-4 times with acetonitrile. Suspend the filter cake in 500 ml of hot ethanol, and add saturated ethanol solution of sodium bicarbonate until the pH value is 7.5-9.0. Remove the insoluble impurities by filtration, remove part of the ethanol solution by rotary evaporation, recrystallize after cooling, and filter to obtain the brown-red sodium tanshinone IIA sulfonate product.

Embodiment 2

[0027] Add 200 grams of crude tanshinone extract (tanshinone IIA content is about 50%) into 1000 ml of ethyl acetate solvent, and then add 100 grams of sulfur trioxide-diisopropylethylamine complex with stirring. The reaction solution was heated to reflux with stirring, and cooled to room temperature after the reaction. The reaction solution was filtered, and the filter cake was washed 3-4 times with ethyl acetate. Suspend the filter cake in 300 ml of water, add 50% aqueous sodium hydroxide solution to pH 7.5-9.0. Remove insoluble impurities by filtration, remove part of the aqueous solution by rotary evaporation, recrystallize after cooling, and filter to obtain the brown-red sodium tanshinone IIA sulfonate product.

Embodiment 3

[0029] Add 200 grams of tanshinone crude extract (tanshinone IIA content is about 80%) to 1000 ml of dichloroethane solvent, and then add 120 grams of sulfur trioxide-pyridine complex with stirring. The reaction solution was heated to 140 degrees Celsius and stirred, and cooled to room temperature after the reaction was completed. The reaction solution was filtered, and the filter cake was washed 3-4 times with dichloroethane. Suspend the filter cake in 600 ml of acetone, and add saturated aqueous sodium carbonate solution until the pH value is 7.5-9.0. Remove insoluble impurities by filtration, remove part of the acetone solution by rotary evaporation, recrystallize after cooling, and filter to obtain the brown-red sodium tanshinone IIA sulfonate product.

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Abstract

The invention provides a method for preparing tanshinone IIA sodium sulfonate by directly adopting a tanshinone crude extract. According to the method, the tanshinone crude extract is directly subjected to sulfonation reaction in an organic solvent by using a sulfur trioxide or sulfur trioxide complex, after the reaction is ended, a reaction solution is filtrated, washing is carried out by using an organic solvent so as to remove unreacted impurities in the tanshinone crude extract and other impurities which can be dissolved in the organic solvent, and the obtained filter cake is dissolved and then is converted into tanshinone IIA sodium sulfonate by using a sodium containing reagent. The method has the advantages that the sulfonation reaction is carried out by adopting an environmental-friendly reagent instead of chemical reagents, such as concentrated sulfuric acid, acetic acid, acetic anhydride and the like, which cause serious environmental pollution. Meanwhile, the reaction is carried out by directly adopting the tanshinone crude extract as a raw material, so that the cost caused by adopting high-purity tanshinone IIA as the raw material is reduced, byproducts of the obtained product are few, and the yield and purity of the product are high.

Description

field of invention [0001] The invention relates to a method for directly using the crude extract of tanshinone as a raw material to prepare sodium tanshinone IIA sulfonate, that is, sulfonating the crude extract of tanshinone with sulfur trioxide or a sulfur trioxide compound in an organic solvent, and the reaction ends Finally, the reaction solution is filtered and washed with an organic solvent to remove unreacted raw materials and other soluble impurities in the organic solvent. After the obtained filter cake is dissolved, it is converted into sodium tanshinone IIA sulfonate with a sodium-containing reagent. Background technique [0002] Tanshinone IIA is a fat-soluble active ingredient extracted from the traditional Chinese medicine Danshen (Slavia miltiorrhiza Bge.) of the Labiatae family. Its metabolites in the body can participate in various biochemical reactions of the body and exhibit various pharmacological effects. It is often used in the treatment of angina pecto...

Claims

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Application Information

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IPC IPC(8): C07J73/00
Inventor 夏成峰李大山
Owner 华药控股有限公司
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