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Method for preparing spherosin

A technology of swainsonine and methanol, applied in the direction of organic chemistry and the like, can solve the problems of small preparation amount and complicated industrial operation, and achieve the effects of reducing dissolution, simplifying purification steps and being beneficial to purification.

Inactive Publication Date: 2012-01-25
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method is complicated in industrial operation and the preparation amount is small

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The raw material of bonnet grass is crushed to 20 meshes, take 2kg, add 10L80% methanol, heat to 45°C and extract for 3 hours, filter the liquid, add 10L80% methanol for extraction for 3 hours, combine the extracts and concentrate until there is no alcohol, add an appropriate amount of water to disperse , filtered, the filtrate was added to a HPD100 macroporous resin column, the liquid through the column was collected, concentrated under reduced pressure, the concentrated solution was added with ammonia water to adjust the pH to 10, and then 200 mL of dichloromethane was added for extraction, extracted twice, and the extract was concentrated to a small volume. Take chloroform, methanol, butanol, and water solvents, mix them in a ratio of 27:1:17:12, take the upper phase as the mobile phase, and the lower phase as the stationary phase, inject the stationary phase into the high-speed countercurrent chromatography column, turn on the machine, adjust The speed of the main ma...

Embodiment 2

[0018] Raw materials of locoweed are crushed into 40 meshes, take 4kg, add 30L of 90% methanol, heat to 55°C and extract for 2 hours, filter the liquid, add 20L of 90% methanol for extraction for 2 hours, combine the extracts and concentrate until alcohol-free, add appropriate amount of water to disperse , filter, add the filtrate to the AB-8 macroporous resin column, collect the liquid through the column, concentrate under reduced pressure, add ammonia water to the concentrated solution to adjust the pH to 12, then add 300mL dichloromethane for extraction, extract twice, and concentrate the extract to a small volume . Take chloroform, methanol, butanol, and water solvents, mix them in a ratio of 30:1:17:12, take the upper phase as the mobile phase, and the lower phase as the stationary phase, inject the stationary phase into the high-speed countercurrent chromatography column, turn on the machine, adjust The speed of the main machine is 950r / min, the flow rate is 4ml / min, the...

Embodiment 3

[0020] Crazy grass raw material is crushed into 60 mesh, take 10kg, add 60L90% methanol, heat to 50°C and keep it for extraction for 2 hours, filter the liquid, add 60L90% methanol for extraction for 2 hours, combine the extracts and concentrate until alcohol-free, add appropriate amount of water to disperse , filter, add the filtrate to the HZ816 macroporous resin column, collect the liquid through the column, concentrate under reduced pressure, add ammonia water to the concentrated solution to adjust the pH to 11, then add 300mL dichloromethane for extraction, extract 3 times, and concentrate the extract to a small volume. Take chloroform, methanol, butanol, and water solvents, mix them in a ratio of 25:1:17:12, take the upper phase as the mobile phase, and the lower phase as the stationary phase, inject the stationary phase into the high-speed countercurrent chromatography column, turn on the machine, adjust The speed of the main machine is 900r / min, and the flow rate is 2ml...

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PUM

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Abstract

The invention provides a method for preparing spherosin. The method comprises the steps of: crushing a crazyweed raw material; adding methanol in the crazyweed raw material for soaking and extracting; concentrating an extracted solution; deconcentrating by adding a proper amount of water; filtering; adding a macroporous resin column in a filtrate; collecting liquid passing through the column, depressurizing and concentrating until the liquid is nearly dried; adding a proper amount of ammonia water in a concentrated liquid; extracting through methylene chloride, and concentrating an extract liquid to a small volume; and separating by adopting a high-speed countercurrent chromatography, collecting an eluate and recovering a reagent, and vacuum-drying to obtain a product. The method provided by the invention has the characteristics of simple technological operation, no loss of products, large preparation quantity and small pollution.

Description

technical field [0001] The invention belongs to the field of separation of natural products, in particular to a preparation method of swainsonine. Background technique [0002] Swainsonine is an indole alkaloid, its chemical name is 1,2,8-trihydroxyoctahydroindorazidine, and its high-purity swainsonine is a white needle-like crystal with a melting point of 144°C-145°C. Molecular formula C 8 h 15 NO 3 , molecular weight 173, acid dissociation constant 7.4, soluble in water. [0003] Swainsonine, a toxic component originally isolated from the gray horse soya bean, is the main component of locoweed that causes animal poisoning. Modern medical research shows that swainsonine can activate the cell binding activity of animal peritoneal phagocytes, thereby inhibiting tumor cells, which is of great significance for the treatment of tumors, infectious diseases, and immunosuppressive diseases. The latest research shows that swainsonine can effectively reverse the bone marrow supp...

Claims

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Application Information

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IPC IPC(8): C07D471/04
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司