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Preparation method of postassium dehydroandrographolide succinate

A technology of Chuanhuning and dehydrated Andrographis paniculata, which is applied in the field of preparation of Chuanhuning, can solve the problems that the efficacy and stability of Chuanhuning are difficult to guarantee, and the residual amount of impurities is high, so as to ensure the efficacy and stability of the medicine, reduce the residual amount, and reduce the content.

Inactive Publication Date: 2019-01-11
CHENGDU TONGDE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Chuanhuning is a good antiviral drug, which has antipyretic and anti-inflammatory effects. It is widely used clinically for viral pneumonia and upper respiratory tract infections. sex is difficult to guarantee

Method used

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  • Preparation method of postassium dehydroandrographolide succinate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A preparation method of Chuanhuning, comprising the following steps:

[0022] S1. Mix 100g of dried andrographolide and 100g of succinic anhydride, add it to a three-necked flask equipped with a stirrer, a reflux condenser and a thermometer, then add 100ml of pyridine to the three-necked flask, and stir to raise the temperature to reflux under the protection of nitrogen. state (pyridine boiling point 115°C), temperature controlled reaction for 4 hours, after the reaction was completed, cooled to 65°C to obtain a reaction liquid;

[0023] S2. Pour the reaction solution obtained in step S1 into 2000ml hydrochloric acid solution and stir to disperse. The pH value of the hydrochloric acid solution is 5 to obtain a solid substance (yellow);

[0024] S3, the solid matter obtained in step S2 is washed, filtered, soaked in pure water for 4 hours, put into a drying oven and dried at 50° C. for 5 hours to obtain a crude product of dehydrated andrographolide disuccinate half ester...

Embodiment 2

[0029] A preparation method of Chuanhuning, comprising the following steps:

[0030] S1. Mix 100g of dried andrographolide and 100g of succinic anhydride, add it to a three-necked flask equipped with a stirrer, a reflux condenser and a thermometer, then add 100ml of pyridine to the three-necked flask, and stir to raise the temperature to reflux under the protection of nitrogen. state (pyridine boiling point 115°C), temperature controlled reaction for 6 hours, after the reaction was completed, cooled to 75°C to obtain a reaction solution;

[0031] S2. Pour the reaction solution obtained in step S1 into 2000ml hydrochloric acid solution and stir to disperse. The pH value of the hydrochloric acid solution is 6 to obtain a solid substance (yellow);

[0032] S3, the solid matter obtained in step S2 is washed, filtered, soaked in pure water for 4 hours, put into a drying oven and dried at 50° C. for 5 hours to obtain a crude product of dehydrated andrographolide disuccinate half est...

Embodiment 3

[0037] A preparation method of Chuanhuning, comprising the following steps:

[0038] S1. Mix 100g of dried andrographolide and 100g of succinic anhydride, add it to a three-necked flask equipped with a stirrer, a reflux condenser and a thermometer, then add 100ml of pyridine to the three-necked flask, and stir to raise the temperature to reflux under the protection of nitrogen. state (pyridine boiling point 115°C), temperature controlled reaction for 5 hours, after the reaction was completed, cooled to 70°C to obtain a reaction solution;

[0039] S2. Pour the reaction solution obtained in step S1 into 2000ml hydrochloric acid solution and stir to disperse. The pH value of the hydrochloric acid solution is 5.5 to obtain a solid substance (yellow);

[0040] S3, the solid matter obtained in step S2 is washed, filtered, soaked in pure water for 4 hours, put into a drying oven and dried at 50° C. for 5 hours to obtain a crude product of dehydrated andrographolide disuccinate half e...

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Abstract

The invention discloses a preparation method of postassium dehydroandrographolide succinate, wherein the preparation method comprises the following steps: adding andrographolide and succinic anhydrideinto pyridine, under the protection of inert gas, stirring and heating up to a reflux state, carrying out a temperature-controlled reaction for 4 h-6 h, cooling to 65 DEG C-75 DEG C after the reaction is finished, pouring into a hydrochloric acid solution with the pH value of 5-6, stirring and dispersing, washing, filtering, soaking, and drying to obtain a crude product; adding the crude productinto an alcoholic solvent, dissolving, adding activated carbon, heating and refluxing for 30 min and filtering to obtain a filtrate; cooling the filtrate to -25 DEG C to -20 DEG C, and removing the alcoholic solvent with a vacuum pump at the temperature of 0 DEG C, to obtain a refined product; and adding the refined product into an ethanol solution, dissolving, heating to 30 DEG C, slowly dropwiseadding a potassium bicarbonate saturated solution, carrying out heat preservation stirring until no bubbles are generated no longer, naturally cooling for 2 h, then filtering, and drying to obtain postassium dehydroandrographolide succinate. The prepared postassium dehydroandrographolide succinate has less residual quantity of pyridine, so as to ensure the pharmacological function and stability of the product.

Description

technical field [0001] The invention belongs to the technical field of medicine preparation, in particular to a preparation method of Chuanhuning. Background technique [0002] Chuanhuning is a good antiviral drug, which has antipyretic and anti-inflammatory effects. It is widely used clinically for viral pneumonia and upper respiratory tract infections. Sex is hard to guarantee. Contents of the invention [0003] In order to solve the above-mentioned problems existing in the prior art, the present invention provides a preparation method of Chuanhuning. The residual amount of pyridine in the Chuanhuning prepared by the preparation method is less, thereby ensuring the efficacy and stability of the product. [0004] The technical scheme adopted in the present invention is: [0005] A preparation method of Chuanhuning, comprising the following steps: [0006] S1. Add andrographolide and succinic anhydride to pyridine, under the protection of an inert gas, stir and heat up...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/60
CPCC07D307/60
Inventor 李晓琳范伟川张庆坤张利蓉
Owner CHENGDU TONGDE PHARMA
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