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A kind of preparation method of sulfonated dehydroabietic acid salt

A technology of dehydroabietic acid and bismuth abietic acid, which is applied in the field of medicine for diseases, can solve the problems of high temperature required for the reaction, increase of related substances, and low production efficiency, so as to reduce the generation of by-products, increase the reaction yield, and reduce the raw material cost effect

Active Publication Date: 2015-08-26
北京海一药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the prior art, sulfonated dehydroabietic acid is prepared into sulfonated dehydroabietic acid salt. The reaction solvent is a C1-6 fatty alcohol, a solvent in water, DMF and DMSO, and the reaction system is a liquid-homogenization reaction , not conducive to the reaction, easy to form a mixture
And the reaction requires high temperature, resulting in a significant increase in related substances, low production efficiency, and high energy consumption, so this preparation method is not very meaningful in industrial production

Method used

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  • A kind of preparation method of sulfonated dehydroabietic acid salt
  • A kind of preparation method of sulfonated dehydroabietic acid salt
  • A kind of preparation method of sulfonated dehydroabietic acid salt

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Experimental program
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Effect test

Embodiment 1

[0018] Study on the solubility of bismuth nitrate pentahydrate

[0019] (1) Take 500 mg of bismuth nitrate pentahydrate, add 5 ml of glycerin: water = 1:1 mixed solution, heat it slightly, all the salt will be dissolved, and the salt will naturally fall to room temperature overnight without solid precipitation.

[0020] (2) Take 500 mg of bismuth nitrate pentahydrate, add 5 ml of glycerin: water = 1:2 mixed solution, ultrasonically dissolve all, and let it stand overnight. The solution is clear and no solid is precipitated.

[0021] (3) Take 500 mg of bismuth nitrate pentahydrate and add 5 ml of glycerol:water = 1:3 mixed solution, which can be quickly dissolved without ultrasound. After standing overnight, the solution is clear without solid precipitation.

[0022] (4) Take 500 mg of bismuth nitrate pentahydrate, add 5 ml of glycerol: water = 1:4 mixed solution, ultrasonically quickly dissolve, leave it overnight, the solution has a small amount of solid precipitation.

[0023] (5) Tak...

Embodiment 2

[0029] Dissolve 1.654 kg of bismuth nitrate pentahydrate in a mixed solvent of 28L glycerol: water = 1:3. After dissolving completely, filter, and then dissolve 1.42 kg of sulfonated dehydroabietic acid in 2.8L of 75% ethanol. , Was dropped into bismuth nitrate aqueous glycerol solution, reacted for 30 minutes, centrifuged, and then beaten with pure water 25L*3 times, and the filter cake was dried under vacuum at 60°C for 24 hours to obtain 1.6 kg of sulfonated bismuth dehydroabietic acid salt, which was detected by HPLC The purity is 99.90%.

Embodiment 3

[0031] Dissolve 45g of bismuth nitrate pentahydrate in a mixed solvent of 800mL of glycerol: water = 1:3. After the solution is completely dissolved, filter, and then dissolve 40g of sulfonated dehydroabietic acid in 80mL of 75% ethanol. In the glycerol aqueous solution of bismuth nitrate, react for 30 minutes, centrifuge, and then be beaten with 800 mL of pure water for 3 times. The filter cake is dried under vacuum at 60°C for 24 hours to obtain 43.3 g of sulfonated bismuth dehydroabietic acid salt. Its purity is 99.92 by HPLC. %.

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Abstract

The invention discloses a method for preparing a sulfonated dehydroabietic acid salt. The method is characterized by comprising the following steps: dissolving bismuth nitrate pentahydrate into a mixed solvent of glycerol and water of which the ratio is 1:3 at room temperature; filtering after fully dissolving; dissolving sulfonated dehydroabietic acid into ethanol; dripping into the glycerol water solution of bismuth nitrate after fully dissolving; reacting at room temperature for 30 minutes; centrifuging, and pulping by using pure water; drying a filter cake at 60 DEG C in vacuum for 24 hours, so as to obtain sulfonated dehydroabietic acid bismuth.

Description

Technical field [0001] The invention relates to a preparation method of sulfonated dehydroabietic acid and a medicine that can be used to treat diseases such as peptic ulcer, acute and chronic gastritis, erosive gastritis and the like. Background technique [0002] Peptic gastric ulcer is an ulcer disease caused by the digestive action of gastric acid and pepsin. It mostly occurs in the stomach and duodenum. This type of disease is prone to repeated attacks and easily causes cancer. Commonly used therapeutic drugs include antacid sodium bicarbonate, aluminum phosphate, anti-gastric acid secretion drugs secretin, cimetidine, ranitidine, gastric mucosal protector sucralfate, compound bismuth subnitrate, teprenone, and Motive drugs metoclopramide, domperidone, mosapride, etc. Too much use of antacids can easily cause hypochlorhydria, which will significantly reduce the digestive activity of pepsin and cause indigestion; gastric mucosal protective agents such as gastric ketone can c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/58C07C303/32A61K31/255A61P1/04
Inventor 张在富吴浩山许馨文
Owner 北京海一药业有限公司