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Method for preparing high purity 9,11-dehydromanogenin

A high-purity technology of hydromanogenin, which is applied in the field of preparation of 9 with a mass percentage purity greater than 95%, which can solve the problems of difficult mass production, cumbersome operation, and low yield, and achieve reduced dosage, simplified process, and reduced cost Effect

Inactive Publication Date: 2012-09-19
SHANGHAI JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The yield of this method is extremely low, only 9 / 100,000, and the operation is cumbersome, requiring steps such as sulfuric acid hydrolysis, saponification, multiple extractions, column chromatography, recrystallization, etc., the cost is high, and benzene, chloroform, Toxic organic solvents such as methanol
This method is difficult to prepare a large amount of 9,11-dehydromanogenin

Method used

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  • Method for preparing high purity 9,11-dehydromanogenin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] This embodiment 1 is implemented under the following conditions of implementation and technical requirements:

[0026] 1) 500g of the rhizome of Calyx aurantiae, crushed into a coarse powder, add 2500mL of 70(v / v)% industrial ethanol to reflux for extraction for 2h, filter, recover ethanol from the filtrate (for the next extraction), and obtain extract; repeat the above operation 1 time, combined 2 times of the gained extract to obtain alcoholic extract 117g;

[0027] 2) Take the alcohol extract, add 300mL of water to suspend, then extract 3 times with 300mL of dichloromethane, combine the dichloromethane layers, and recover the dichloromethane under reduced pressure (for the next extraction);

[0028] 3) The water layer after dichloromethane extraction was continued to be extracted 3 times with 300 mL of water-saturated n-butanol, the n-butanol layers were combined, and n-butanol was recovered (for the next extraction), to obtain 42 g of total saponins;

[0029] 4) Di...

Embodiment 2

[0032] This embodiment 2 is implemented under the following conditions of implementation and technical requirements:

[0033] 1) 500 g of purple calyx leaves, crushed into coarse powder, added 4000 mL of 95 (v / v)% industrial ethanol for reflux extraction for 2 hours, filtered, recovered ethanol from the filtrate (for the next extraction) to obtain extract. Repeat the above operation, combine the extracted extract obtained twice to obtain 159g of alcoholic extract;

[0034] 2) Take the alcohol extract, add 350mL of water to suspend, then extract 3 times with 350mL of dichloromethane, combine the dichloromethane layers, and recover the dichloromethane (for the next extraction);

[0035] 3) The water layer after dichloromethane extraction was continued to be extracted 3 times with 350 mL of water-saturated n-butanol, the n-butanol layer was combined, and n-butanol was recovered (for the next extraction) to obtain 36 g of total saponins;

[0036] 4) Dissolve the total saponins in...

Embodiment 3

[0039] This embodiment 3 is implemented under the following conditions of implementation and technical requirements:

[0040] 1) 500g of the whole plant of Violet Calyx, crushed into a coarse powder, added 3500mL of 80(v / v)% industrial ethanol for reflux extraction for 2h, filtered, recovered ethanol from the filtrate (for the next extraction) to obtain extract. The above operation was repeated once, and the extracted extracts obtained from the two extractions were combined to obtain 120 g of alcoholic extracts.

[0041] 2) Take the alcohol extract, add 300mL of water to suspend, then extract 3 times with 300mL of dichloromethane, combine the dichloromethane layers, and recover the dichloromethane under reduced pressure (for the next extraction).

[0042] 3) The water layer after dichloromethane extraction was continued to be extracted 3 times with 300 mL of water-saturated n-butanol, the n-butanol layers were combined, and n-butanol was recovered (for the next extraction) to ...

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Abstract

The invention relates to a method for preparing high purity 9,11-dehydromanogenin in the technical field of chemical purification. The high purity 9,11-dehydromanogenin is prepared from a common ornamental plant of Hosta ventricosa through two-phase acid hydrolysis. The method is not subject to operations, such as column chromatography, saponification, and the like, and has the advantages that the raw material is rich and low in price and easily obtained, the process is simple, an organic solvent can be recycled and has low cost, an obtained product has high purity and yield, and the like.

Description

technical field [0001] The invention relates to a method in the field of chemical purification technology, in particular to a method for preparing 9,11-dehydromanogenin with a mass percentage purity greater than 95%. Background technique [0002] 9,11-dehydromannogenin (9,11-dehydromanogenin) is a spirane sterane component, currently only found in Agave, Furcraea and Hosta, Liliaceae This component is found in some plants. Its structural formula is as follows: [0003] [0004] 9,11-Dehydromanogenin has significant anti-inflammatory and anti-tumor effects, and can also be further synthesized through structural modification to further synthesize glucocorticoid drugs with wide range of uses and good effects, such as cortisone, prednisone, etc. , so the preparation of 9,11-dehydromannogenin is of great significance. [0005] Although 9,11-dehydromanogenin exists in Agave, Vanilla and Hosta, the content is low and it is difficult to prepare in large quantities. If it is d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J71/00
Inventor 李晓波王梦月黄文武李锐
Owner SHANGHAI JIAOTONG UNIV
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