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Preparation method of hyperbranched poly(beta-cyclodextrin) containing azide group

A technology of hyperbranched polycyclodextrin, which is applied in the field of preparation of hyperbranched polycyclodextrin, can solve the problem of single inclusion guest molecules, and achieve the effect of simplified steps and high controllability

Inactive Publication Date: 2011-08-17
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the deficiencies of the prior art in terms of terminal group modification, functionalization, and inclusion of a single guest molecule, the present invention adopts an improved dual-monomer method and the principle of hydrosilylation to provide a novel azide-containing A Simple and Efficient Method for Group Hyperbranched Poly(β-cyclodextrin)

Method used

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  • Preparation method of hyperbranched poly(beta-cyclodextrin) containing azide group
  • Preparation method of hyperbranched poly(beta-cyclodextrin) containing azide group
  • Preparation method of hyperbranched poly(beta-cyclodextrin) containing azide group

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Experimental program
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Effect test

Embodiment 1

[0020] Weigh 3g of six-position monosubstituted p-tosylated β-cyclodextrin, 0.193g of potassium iodide, and 1.52g of sodium azide in a dry single-necked flask, add 10mL of N,N-dimethylformamide as a solvent, Fully dissolve for 0.5 h under nitrogen protection and magnetic stirring. After dissolving the above substances, the resulting system was sealed with nitrogen protection and continued to stir and react at 80° C. for 26 h. Add 30 mL of distilled water to the solution after the reaction and continue to stir for 20 min, and filter the obtained turbid solution with a G4 sand core funnel to remove insoluble matter to obtain a transparent solution. Gradually add 60 mL of acetone-water blend solvent (the volume ratio of acetone to water is 2:1) to the transparent solution, slowly precipitate the precipitate, put it in the refrigerator at 4°C for 24h, filter out the solid product, and dry it in vacuum at 25°C In 3 days, 2.4 g of six-position monosubstituted azide β-cyclodextrin m...

Embodiment 2

[0026] Add 6g of six-position monosubstituted p-toluenesulfonylated β-cyclodextrin, 0.386g of potassium iodide, 3.05g of sodium azide and 15mL of N,N-dimethylformamide into a dry one-necked flask, under nitrogen protection, magnetic stirring Fully dissolved under the conditions of 0.5h. After dissolving the above substances, the resulting system was sealed with nitrogen protection and continued to stir and react at 85° C. for 25 h. After the reaction was completed, 60 mL of distilled water was added to the solution and continued to stir for 25 min. The obtained turbid solution was filtered with a G4 sand core funnel to remove insoluble matter to obtain a transparent solution. Gradually add 120mL of acetone-water blend solvent (the volume ratio of acetone to water is 2:1) to the transparent solution, and the precipitate slowly precipitates out, and the solid product is filtered out after standing at 4°C in the refrigerator for 24h, and the obtained solid product is 30°C Vacuum...

Embodiment 3

[0030] Add 10g of six-position monosubstituted p-toluenesulfonylated β-cyclodextrin, 0.643g of potassium iodide, 5.07g of sodium azide and 30mL of N,N-dimethylformamide into a dry single-necked flask, under nitrogen protection, magnetic stirring Fully dissolved under the conditions of 0.5h. After dissolving the above substances, the resulting system was sealed with nitrogen protection and continued to stir and react at 90° C. for 24 h. Add 100 mL of distilled water to the solution after the reaction, continue to stir for 30 min, filter the obtained cloudy solution with a G4 sand core funnel to remove insoluble matter, and obtain a transparent solution. Gradually add 180 mL of acetone-water blend solvent (the volume ratio of acetone to water is 2:1) to the transparent solution, and precipitate slowly. After standing in the refrigerator at 4°C for 24h, the solid is filtered out, and vacuum-dried at 30°C for 5 Tian obtained 7.1g of six-position monosubstituted azide β-cyclodextr...

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Abstract

The invention discloses a preparation method of a hyperbranched poly(beta-cyclodextrin) containing an azide group. The preparation method comprises the following steps of: firstly, preparing a hexa-monosubstituted azido beta-cyclodextrin monomer from hexa-monosubstituted paratoluene sulfonylated beta-cyclodextrin, potassium iodine and sodium azide; secondly, preparing a polysilicon hydrogenated beta-cyclodextrin monomer containing hexa-mono azide from the hexa-monosubstituted azido beta-cyclodextrin monomer, dimethyl dichlorosilane and pyridine; and lastly, preparing the hyperbranched poly(beta-cyclodextrin) containing an azide group from the polysilicon hydrogenated beta-cyclodextrin monomer containing hexa-mono azide and divinyl tetramethyldisiloxane. By adopting the method, complex steps in monomer synthesis are simplified, the branching coefficient of the poly(beta-cyclodextrin) and the proportion of cyclodextrin molecules have higher controllability, and the outer end of the poly(beta-cyclodextrin) can be quickly modified by effectively utilizing a click chemistry reaction.

Description

technical field [0001] The invention belongs to the field of polymer material synthesis and relates to a preparation method of hyperbranched polycyclodextrin. Background technique [0002] Designing and synthesizing hyperbranched molecular hosts with functional groups is an effective means to prepare functional biological macromolecules, pharmaceutical macromolecules and macromolecular prodrugs. [0003] Document 1 "Wei Tian, ​​Xiaodong Fan, Jie Kong et al. Cyclodextrin-Based Hyperbranched Polymers: Molecule Design, Synthesis, and Characterization. Macromolecules, 2009, 42(3): 640-651" discloses a modified β -Cyclodextrin is a monomer, a method for synthesizing novel hyperbranched poly(β-cyclodextrin) by hydrosilylation reaction under thermal or ultraviolet light conditions. This method can improve the molecular inclusion ability of hyperbranched polymers, but the preparation process takes a long period, and it is difficult to carry out more in-depth end group modification....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/16C08G77/50
Inventor 田威魏晓莹张卫红孔杰
Owner NORTHWESTERN POLYTECHNICAL UNIV
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