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Ultrasonic wave assistant-catalyzed synthesis of grifolan sulphate

A Grifola frondosa polysaccharide, ultrasonic-assisted technology, applied in the field of polysaccharide structure modification of traditional Chinese medicine, can solve the problems of explosive danger, high operation requirements, explosion hazard, etc., and achieve the effect of increasing the degree of substitution, mild and controllable reaction conditions, and fast reaction speed

Inactive Publication Date: 2014-05-28
BEIJING UNION UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this patent document, chlorosulfonic acid is used as a sulfonating reagent in the synthesis of polysaccharide sulfate, but chlorosulfonic acid is a strong oxidizing agent, which will decompose violently when exposed to water, release a large amount of heat, have dense smoke, and have explosive danger. restricted chemicals
The preparation of sulfonating agent by the reaction of chlorosulfonic acid with pyridine or formamide needs to be carried out in an ice bath, and the chlorosulfonic acid needs to be added dropwise slowly, and the reaction system must be strictly controlled not to contain water. The operation requirements are high, and improper control is prone to explosion hazards

Method used

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  • Ultrasonic wave assistant-catalyzed synthesis of grifolan sulphate
  • Ultrasonic wave assistant-catalyzed synthesis of grifolan sulphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Weigh 6.0g of sulfur trioxide-pyridine complex in a reactor equipped with condensation, stirring, and heating devices, add 60mL of pyridine therein, and stir at room temperature to fully dissolve the sulfur trioxide-pyridine complex to obtain ester Chemical homogeneous liquid A.

[0034] (2) Weigh 3.0 g of Grifola frondosa polysaccharide that has undergone decolorization and fractional purification, add 45 mL of N, N-dimethylformamide (DMF) to it, and ultrasonically swell for 60 min at a frequency of 40 Hz in an ultrasonic reactor , to obtain Grifola frondosa polysaccharide dispersion B.

[0035] (3) 1.0 g of 4-dimethylaminopyridine (DMAP) was dissolved in the Grifola frondosa polysaccharide dispersion B at room temperature to obtain the Grifola frondosa polysaccharide dispersion C containing DMAP.

[0036] (4) Esterification reaction: Slowly add the Grifola frondosa polysaccharide dispersion C obtained in step (3) into A, react in an oil bath at 50°C for 3 hours, ...

Embodiment 2

[0040] (1) Weigh 9.0g of sulfur trioxide-pyridine complex in a reactor equipped with condensation, stirring and heating devices, add 60mL of pyridine therein, and stir at room temperature to fully dissolve the sulfur trioxide-pyridine complex to obtain ester Chemical homogeneous liquid A.

[0041] (2) Weigh 3.0 g of Grifola frondosa polysaccharide that has undergone decolorization and fractional purification, add 45 mL of N, N-dimethylformamide (DMF) to it, and ultrasonically swell for 40 min at a frequency of 80 Hz in an ultrasonic reactor , to obtain Grifola frondosa polysaccharide dispersion B.

[0042] (3) 1.0 g DMAP was dissolved in the Grifola frondosa polysaccharide dispersion B at room temperature to obtain the Grifola frondosa polysaccharide dispersion C containing DMAP.

[0043] (4) Esterification reaction: Slowly add the Grifola frondosa polysaccharide dispersion C obtained in step (3) into A, react in an oil bath at 60°C for 3 hours, after the reaction is complete...

Embodiment 3

[0046] (1) Weigh 12g of sulfur trioxide-pyridine complex in a reactor equipped with condensation, stirring, and heating devices, add 60mL of pyridine thereto, and stir at room temperature to fully dissolve the sulfur trioxide-pyridine complex to obtain esterification Agent homogeneous liquid A.

[0047] (2) Weigh 3 g of Grifola frondosa polysaccharide that has been decolorized and fractionated and purified, add 45 mL of N, N-dimethylformamide (DMF) to it, and in an ultrasonic reactor, ultrasonically swell for 60 min at a frequency of 60 Hz to obtain Grifola frondosa polysaccharide dispersion B.

[0048] (3) 1.0 g DMAP was dissolved in the Grifola frondosa polysaccharide dispersion B at room temperature to obtain the Grifola frondosa polysaccharide dispersion C containing DMAP.

[0049] (4) Esterification reaction: Slowly add the Grifola frondosa polysaccharide dispersion C obtained in step (3) into A, react in an oil bath at 70°C for 4 hours, after the reaction is completed, ...

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Abstract

The invention discloses a method for ultrasonic wave assistant-catalyzed synthesis of grifolan sulphate. According to the method, the grifolan is used as a raw material, and sulfur trioxide-pyridine is used as a sulfonating agent, under the catalytic action of 4-dimethylaminopyridine, the grifolan sulphate can be prepared, further, the method includes the step of ultrasound swelling of grifolan in N,N-dimethylformamide. According to the method, as the synthesis of grifolan sulphate is realized through the ultrasonic wave assistant-catalysis method, the esterification temperature is reduced, the esterification time is shortened, and the degree of substitution of sulfuric acid groups is improved by 1.07-2.13; with the adoption of the method provided by the invention, the reaction condition is safe and controllable, and the reaction speed is higher.

Description

technical field [0001] The invention relates to a method for ultrasonically assisted-catalyzed synthesis of Grifola frondosa polysaccharide sulfate ester, which belongs to the technical field of structure modification of traditional Chinese medicine polysaccharides. Background technique [0002] The various activities of human cells are closely related to sugars. Polysaccharides are another important biological macromolecule besides proteins and nucleic acids in organisms. They have non-specific immune enhancement functions, can improve the body's immunity, and have anti-infection and anti-tumor , anti-oxidation and prevention and treatment of viral hepatitis, AIDS and other functions. The biological activity of polysaccharides is closely related to its structure, molecular weight, solubility and other factors. In particular, the introduction of certain chemical groups can change the flexibility and spatial structure of sugar chains, thereby causing changes in the solubility...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/00
Inventor 刘红梅
Owner BEIJING UNION UNIVERSITY
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