Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of cyclodextrin terminated star-shaped polymer

A star-shaped polymer and cyclodextrin technology, which is applied in the field of star-shaped polymer preparation, can solve problems such as lack, and achieve the effects of expanding types, expanding application range, and mild reaction conditions

Active Publication Date: 2018-12-04
ZHONGBEI UNIV
View PDF5 Cites 6 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the research on cyclodextrin-terminated star polymers is still lacking, so it is necessary to design and prepare cyclodextrin-terminated star polymers

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of cyclodextrin terminated star-shaped polymer
  • Preparation method of cyclodextrin terminated star-shaped polymer
  • Preparation method of cyclodextrin terminated star-shaped polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1: Preparation of six-arm star polymer (i)

[0023] Under anhydrous and oxygen-free operation, weigh 0.2543 g (1 mmol) of dipentaerythritol into a 50 mL eggplant-shaped flask, then add ε-caprolactone 13.30 mL, stir magnetically for 10 minutes, and then add the catalyst containing stannous isooctanoate 0.1 mL of toluene solution 20 mL, and stirred until the solid was completely dissolved; the reaction was gradually heated to 100 ° C, and continued to react at this temperature for 24 h; after the reaction was completed, the reaction solution was cooled to room temperature, and then the mixture was dripped A white solid was precipitated in methanol. After filtration, the filter cake was washed three times with methanol and water, and then dried under vacuum at 40°C for 24 h to obtain the product (i) in the form of white powder.

[0024] Using infrared to analyze its structure, the results are shown in figure 1 , 3443 cm -1 It is the stretching vibration absorp...

Embodiment 2

[0025] Embodiment 2: the preparation of N-BOC-4-aminobenzoic acid

[0026] Weigh 1.00 g of p-aminobenzoic acid and add it to a 50 mL round bottom flask, then add 10 mL of dioxane and 10 mL of distilled water, stir at room temperature for 10 min; add triethylamine in an ice bath at 0°C to adjust the pH of the solution to 9 ~10; Add 3.4 mL of di-tert-butyl dicarbonate in portions within 1.5 h. After the dropwise addition, continue to stir for 2 h under ice bath, and then warm up to room temperature. After reacting for 24 h, the mixture was added dropwise to 100 mL of NaHSO4 solution with a mass fraction of 10%, a large amount of white precipitates were precipitated, the precipitates were collected and washed with water several times, and dried under vacuum at 120 °C to obtain white powdery N -BOC-4 aminobenzoic acid.

Embodiment 3

[0027] Example 3: Preparation of polymer (ii)

[0028] Weigh 1.00 g of six-armed star polymer (ⅰ) and 2 g of N-BOC-4-aminobenzoic acid into a 50 mL round bottom flask, add 30 mL of dichloromethane and stir at room temperature for 10 min; add 2.1742 g dicyclohexylcarbodiimide and 0.0515 g 4-dimethylaminopyridine, the solution gradually became turbid from clear; after continuing to react for 48-72 hours at room temperature, a large amount of white solid precipitated, filtered and poured the filtrate into a round bottom flask , Seal and freeze at -20°C for 2 hours, then filter again, continue to freeze the filtrate, repeat 3-5 times, until no precipitation occurs; concentrate the treated filtrate under reduced pressure until the mixture becomes milky, add methanol to soak, and white precipitates precipitate out, The filter cake was washed several times with methanol and water, respectively, and dried under vacuum at 40°C to obtain the product (ii) as a white solid powder.

[002...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a preparation method of a cyclodextrin terminated star-shaped polymer. The method includes the steps of: under anhydrous and oxygen-free conditions, using dipentaerythritol asthe initiator, using stannous isooctanate as the catalyst to carry out ring-opening polymerization reaction on epsilon-caprolactone so as to obtain six-armed polycaprolactone, and then carrying out esterification reaction on p-aminobenzoic acid to obtain an arylamine terminated six-armed star-shaped polymer, and then further carrying out addition-dehydration reaction with cyclodextrin monoaldehyde, thus obtaining the imine group chained and cyclodextrin terminated six-armed star-shaped polymer. According to the method, cyclodextrin is disposed at the terminal of the star-shaped polymer, the prepared product not only has the three-dimensional structural characteristics of the star-shaped polymer itself, but also can better retain the advantages of the cyclodextrin chamber and cavity surrounding structure, thus enlarging the application range. The invention expands the types of star-shaped cyclodextrin polymers. The preparation method has the advantages of simple operation, mild reactionconditions, and simple product post-treatment, and is beneficial to realization of industrial production.

Description

technical field [0001] The invention relates to a preparation method of a star-shaped polymer whose end is a cyclodextrin, in particular to a method for preparing a star-shaped polymer whose end is a cyclodextrin by reacting a cyclodextrin and a star-shaped polymer, belonging to cyclodextrin Fine modification and star polymer synthesis technology field. Background technique [0002] Star polymer is a hyperbranched structure compound with linear polymer branched chain arms. Compared with linear polymers of the same molecular weight, it not only has a three-dimensional space structure, but also has a smaller viscosity and fluid dynamic radius. Therefore, star polymers It has been used in the carrying of drug molecules and gene delivery. Cyclodextrins (CDs) are compounds with a special ring-shaped cavity structure of "hydrophilic on the outside and hydrophobic on the inside", which can not only contain a variety of organic compound molecules and groups, but also the hydroxyl g...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/91C08G63/08C08B37/16C08G81/00
CPCC08B37/0012C08G63/08C08G63/912C08G81/00
Inventor 李霞谢龙聂小娟李陈成
Owner ZHONGBEI UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com