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A kind of preparation method of galactosylglucan derivative

A technology of galactosyl and dextran, which is applied in the field of preparation of drug carriers, to achieve the effects of easy control of reaction, improvement of reactivity and utilization rate

Active Publication Date: 2016-05-04
昆山京昆油田化学科技有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And the preparation method is simple and easy, and the reaction is easy to control

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Add galactose and dextran (abbreviated as sugars) to triazole nitrate ionic liquid, the mass ratio of galactose to dextran is 2:1, the mass ratio of sugars to ionic liquid is 0.075, and heat at 70°C for 1 hours to dissolve galactose and dextran. Then add thionyl chloride which has a molar ratio of 1.5 to carbohydrates, react at 70°C for 50 min, wash the reaction product with ethanol, centrifuge at 4000r / min for 15 minutes, repeat twice, and then use 4 Wash the reaction product with 1:1 ethanol aqueous solution, centrifuge at 4000r / min for 15 minutes, repeat twice, then wash the reaction product with 1:1 ethanol aqueous solution, centrifuge at 4000r / min for 15 minutes, repeat twice, and finally obtain the sample at 80°C Vacuum dry for 3 hours. After the sample was fully hydrolyzed, the 1 HNMR characterization to determine the degree of substitution (MS) of the sample. The final MS of the sample was 0.0635.

Embodiment 2

[0042] Add galactose and dextran to chloride (1-allyl-3-methylimidazole), the mass ratio of galactose and dextran is 2:1, the mass ratio of carbohydrates and ionic liquid is 0.075, at 70 Heat at °C for 1 hour to dissolve galactose and dextran. Then add thionyl chloride which has a molar ratio of 1.2 to carbohydrates, react at 70°C for 50min, wash the reaction product with ethanol, centrifuge at 4000r / min for 15 minutes, repeat twice, and then use 4 Wash the reaction product with 1:1 ethanol aqueous solution, centrifuge at 4000r / min for 15 minutes, repeat twice, then wash the reaction product with 1:1 ethanol aqueous solution, centrifuge at 4000r / min for 15 minutes, repeat twice, and finally obtain the sample at 80°C Vacuum dry for 3 hours. After the sample was fully hydrolyzed, the 1 HNMR characterization to determine the MS of the sample. The final MS of the sample was 0.0588.

Embodiment 3

[0044] Add galactose and dextran to BmimCl (the mass ratio of galactose to dextran is 2:1, and the mass ratio of carbohydrates to ionic liquid is 0.075), and heat at 70°C for 1 hour to dissolve galactose and dextran . Then add thionyl chloride which has a molar ratio of 1.8 to carbohydrates, and react for 100 min at 60°C. After the reaction, wash the reaction product with ethanol, centrifuge at 4000r / min for 15 minutes, repeat twice, and then use 4 Wash the reaction product with 1:1 ethanol aqueous solution, centrifuge at 4000r / min for 15 minutes, repeat twice, then wash the reaction product with 1:1 ethanol aqueous solution, centrifuge at 4000r / min for 15 minutes, repeat twice, and finally obtain the sample at 80°C Vacuum dry for 3 hours. After the sample was fully hydrolyzed, the 1 HNMR characterization to determine the MS of the sample. The final MS of the sample was 0.2134.

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PUM

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Abstract

The invention relates to a method for preparing galactosyl dextran derivates. The method comprises the following steps: (a) adding galactose and glucosan to ionic liquid, heating and dissolving to obtain an initial solution; (b) adding thionyl chloride to the initial solution obtained in the step (a), and heating to obtain the galactosyl dextran derivates. The reaction system disclosed by the invention is in a homogeneous state, so that, compared with a heterogeneous condition, the reaction activity is greatly improved, and the preparation method disclosed by the invention is simple and feasible, and easy to control reaction.

Description

technical field [0001] The invention relates to a preparation method of a drug carrier, in particular to a preparation method of a galactosyl dextran derivative. Background technique [0002] Glucan is a glucopyranose polymer with the molecular formula (C 6 h 10 o 5 )n, the hemiacetal oxygens of carbons 1, 2, 3, 4, and 6 of the adjacent glucose residues are connected by glucosidic bonds to form a skeleton, and there are two structural forms of α and β positions. Among them, α-glucose Glycans mainly exist in the mucus secreted by certain microorganisms during growth, such as exopolysaccharides produced by fermentation of sucrose by bacteria (such as Leuconostocmesen-teroides), mainly α-1,6- Glucose linked by glycosidic bonds sometimes has α-1,2, α-1,3, α-1,4 branched structures. Scheibler (1869) believed that it was similar to starch and dextrin, so it was named polyglucose, that is, dextran (dextran). [0003] Dextran is currently one of the best plasma substitutes, and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B37/02A61K47/36
Inventor 何建平周静邓明宇彭树华王克尹恒朱明山何俊巩沛鑫
Owner 昆山京昆油田化学科技有限公司
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