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Method for preparing hyper branched supermolecule main block based on modification cyclodextrin

A technology of cyclodextrin and supramolecule, which is applied in the field of preparation of hyperbranched supramolecular body, achieves the effects of low viscosity, novel structure and simple preparation

Inactive Publication Date: 2008-03-12
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If the advantages of highly branched polymers can be combined with cyclodextrins, a new class of supramolecular hosts with important application prospects in the fields of drug delivery and delivery, gene transfection, chemical sensors, and polymer separations can be obtained, However, such highly branched supramolecular hosts have not been reported

Method used

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  • Method for preparing hyper branched supermolecule main block based on modification cyclodextrin

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Step a: Dissolve 30 g of cyclodextrin in 720 ml of aqueous solution, then add 7.8 g of p-toluenesulfonyl chloride, stir at room temperature for 3-5 hours, and the reaction is solid-liquid two-phase. After 3 hours, 120 milliliters of 2.5 mol / liter sodium hydroxide solution was added, the solution became clear, and a little white insoluble matter was removed by filtration. About 9 grams of ammonium chloride was added to adjust the pH to about 8, and white insoluble matter was precipitated in the solution. Place in the refrigerator overnight, filter with suction to obtain a white solid, which is repeatedly recrystallized 3 times. The final product was dried in a vacuum oven at 60 degrees Celsius for 24 hours, and the yield was 16.7%.

[0021] Step b: In N,N-dimethylformamide, 5 g of the prepared p-toluenesulfonylated β-cyclodextrin was dissolved in 20 ml of N,N-dimethylformamide, Add 10 g of hexamethylenediamine and stir for 4 hours at 70°C. Precipitation with 200 mL of...

Embodiment 2

[0024] Step a: Dissolve 30 g of cyclodextrin in 720 ml of aqueous solution, then add 7.8 g of p-toluenesulfonyl chloride, stir at room temperature for 3-5 hours, and the reaction is solid-liquid two-phase. After 3 hours, 120 milliliters of 2.5 mol / liter sodium hydroxide solution was added, the solution became clear, and a little white insoluble matter was removed by filtration. About 9 grams of ammonium chloride was added to adjust the pH to about 8, and white insoluble matter was precipitated in the solution. Place in the refrigerator overnight, filter with suction to obtain a white solid, which is repeatedly recrystallized 3 times. The final obtained product was dried in a vacuum oven at 60 degrees Celsius for 24 hours, and the yield was 16.7%.

[0025] Step b: In N,N-dimethylformamide, 5 g of the prepared p-toluenesulfonylated β-cyclodextrin was dissolved in 20 ml of N,N-dimethylformamide, Add 10 g of hexamethylenediamine and stir for 4 hours at 70°C. Precipitate with 20...

Embodiment 3

[0028] Step a: Dissolve 30 g of cyclodextrin in 720 ml of aqueous solution, then add 7.8 g of p-toluenesulfonyl chloride, stir at room temperature for 3-5 hours, and the reaction is solid-liquid two-phase. After 3 hours, 120 milliliters of 2.5 mol / liter sodium hydroxide solution was added, the solution became clear, and a little white insoluble matter was removed by filtration. About 9 grams of ammonium chloride was added to adjust the pH to about 8, and white insoluble matter was precipitated in the solution. Place in the refrigerator overnight, filter with suction to obtain a white solid, which is repeatedly recrystallized 3 times. The final obtained product was dried in a vacuum oven at 60 degrees Celsius for 24 hours, and the yield was 16.7%.

[0029]Step b: In N,N-dimethylformamide, 5 g of the prepared p-toluenesulfonylated β-cyclodextrin was dissolved in 20 ml of N,N-dimethylformamide, Add 10 g of hexamethylenediamine and stir for 4 hours at 70°C. Precipitate with 200...

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Abstract

The present invention relates to a preparation method for cyclodextrin-based hyperbranched poly-rotaxane in the chemical technology field. The preparation steps are: the cyclodextrin is dissolved in water, wherein methyl benzene sulfonyl chloride p-methyl benzene sulfonic chloride is added. The solution is stirred and filtered to get transparent solution; then chloride ammonia is added into the solution to adjust the pH value; then the solution is crystallized to get tosylation cyclodextrin; tosylation cyclodextrinand the excessive amine monomer are dissolved in the N, N-dimethyl formyl, and react in the heat with the protection of nitrogen. The reaction product is deposited by acetone to get crude amic-substitute cyclodextrin product which is then dissolved by the mixed solution of carbinol and water. Then the solution is deposited for a plurality of times by the acetone to get amic-sinlge-substitute cyclodextrin; the amic-sinlge-substitute cyclodextrin and the Maikeer addition reagent are dissolved in the water or N, N-dimethyl formyl or dimethyl sulfoxide, and are heated for reaction under the protection of nitrogen to get pale yellow or colorless solution; The solution is deposited by methanol or acetone to get pale yellow or colorless powder. The hyperbranched polymer generated by the present invention is of the characteristics of both the hyperbranched polymers and the cyclodextrin.

Description

technical field [0001] The invention relates to a method in the technical field of chemical industry, in particular to a method for preparing a hyperbranched supramolecular body based on modified cyclodextrin. Background technique [0002] Designing and synthesizing host molecules has always been an important field in supramolecular science research and the source of innovative research. It is a research hotspot in this field to seek macrocyclic host molecules that are easy to obtain, have novel structures, and have molecular recognition functions. The emergence often promotes the rapid development of supramolecular science research. Cyclodextrins are one of the most important subjects in supramolecular chemistry. Previously reported cyclodextrin-containing polymeric supramolecular hosts can be classified as cyclodextrin-containing linear polymers or cyclodextrin-crosslinked polymers. [0003] Find through literature search to prior art, linear cyclodextrin is to directly ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/16C08K5/36C08K5/20C08K5/10
Inventor 万会师付灵超屠春来朱新远颜德岳
Owner SHANGHAI JIAO TONG UNIV
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