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A kind of methylated-β-cyclodextrin and its preparation, characterization method and application

A technology of methylation and cyclodextrin, applied in the field of methylation-β-cyclodextrin and its preparation, characterization and application, can solve the tedious, inefficient, and unreported average methylation substitution degree characterization method and other problems, to achieve the effect of accurate test results, low cost of raw materials, and simple and quick measurement methods

Active Publication Date: 2021-05-25
PTG ADVANCED CATALYST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be seen that based on the existing technology, it is cumbersome and inefficient to obtain a relatively accurate average degree of substitution of MBCD, whether it is a standard spectrum or a titration analysis.
[0010] At present, there are few public reports on MBCD with a substitution degree of 12 (±5%), and there is no public report on the characterization method of its average methylation substitution degree

Method used

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  • A kind of methylated-β-cyclodextrin and its preparation, characterization method and application
  • A kind of methylated-β-cyclodextrin and its preparation, characterization method and application
  • A kind of methylated-β-cyclodextrin and its preparation, characterization method and application

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preparation example Construction

[0057] According to the present invention, there is provided a method for preparing methylated-β-cyclodextrin, preferably a method for preparing the methylated-β-cyclodextrin described in the first aspect of the present invention, the method comprising the following steps:

[0058] Step 1. Add BCD into a container filled with aqueous sodium hydroxide solution to obtain a mixed solution.

[0059] In the present invention, in step 1, the sodium hydroxide aqueous solution is obtained by mixing sodium hydroxide and water. When sodium hydroxide is mixed with water, the heat release is obvious, so sodium hydroxide can be added in batches.

[0060] According to the present invention, step 1 includes:

[0061] Step 1.1, adding water to the container, adding sodium hydroxide, preferably adding sodium hydroxide in batches, optionally stirring, to obtain an aqueous sodium hydroxide solution;

[0062] Step 1.2. After the sodium hydroxide aqueous solution is cooled to 20-30°C, add BCD and...

Embodiment 1

[0125] Add 800ml of water to a 2L three-necked flask equipped with a mechanical stirrer, a thermometer, and a constant pressure dropping funnel, and add 141g of sodium hydroxide in batches under stirring. The heat release is obvious, and wait to cool to room temperature;

[0126] Add 200g of BCD, stir well until it is completely dissolved, lower the obtained clear solution to 0°C, slowly add DMS333.38g in 24 batches within 24h, after the dropwise addition, continue to stir at 0°C for 1h, and the reaction system rises to Stir at room temperature overnight, add 25% ammonia water to quench the reaction, and continue stirring for 2 h;

[0127] The resulting solution was adjusted to pH=3.5 with 2M sulfuric acid solution, and transferred to a separatory funnel. Extract with 300ml*2 chloroform, dry with anhydrous sodium sulfate, and filter;

[0128] Rotate the mother liquor to a state close to saturation, add 300ml of n-hexane under stirring, obtain 130g of white powdery solid by su...

Embodiment 2

[0135] Add 1100ml of water to a 2L three-necked flask equipped with a mechanical stirrer, a thermometer, and a constant pressure dropping funnel, and add 211.5g of sodium hydroxide in batches under stirring. The heat release is obvious, and wait to cool to room temperature;

[0136] Add 300g of BCD, stir well until it is completely dissolved, lower the obtained clear solution to 0°C, slowly add 500g of DMS dropwise in 24 batches within 24h, continue to stir at 0°C for 1h, and then raise the reaction system to room temperature and stir Overnight, add 25% ammonia water to quench the reaction, and continue to stir for 2 hours;

[0137] The resulting solution was adjusted to pH=3.5 with 2M sulfuric acid solution, and transferred to a separatory funnel. Extract with 450ml*2 chloroform, dry with anhydrous sodium sulfate, and filter;

[0138] Rotate the mother liquor to a nearly saturated state, add 300ml of n-hexane under stirring, obtain 194g of white powdery solid by suction filt...

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Abstract

The invention discloses a methylated-β-cyclodextrin and its preparation, characterization method and application. The methylated-β-cyclodextrin has an average degree of substitution between 11.4 and 12.6 and a melting range of 181 ~185°C. The methylated-β-cyclodextrin is obtained by methylating BCD with a methylating reagent and crystallizing with an alkane solvent. Preferably, the methylating reagent is DMS. The average degree of methylation substitution of the methylated-β-cyclodextrin prepared by the preparation method provided by the present invention is about 12 (±5%), the yield is high, the preparation method is simple, the conditions are mild, and the average degree of substitution Stable, the characterization method can simply, quickly and accurately characterize the average degree of substitution of MBCD.

Description

technical field [0001] The invention relates to a methylated-β-cyclodextrin and its preparation, characterization method and application. Background technique [0002] Cyclodextrin (abbreviated as CD) is a cyclic oligosaccharide formed by the action of cyclodextrin glycosyltransferase on starch. It has a hydrophilic appearance and a hydrophobic inner cavity. Important host molecules with good biocompatibility are widely used in catalysis, self-assembly, molecular recognition, drug delivery and other fields. [0003] Cyclodextrins are classified into α-cyclodextrin, β-cyclodextrin, and γ-cyclodextrin according to the number of D-glucopyranose units forming the molecule, which contain 6, 7, and 8 glucose units, respectively. [0004] β-cyclodextrin (abbreviated as BCD) is a macrocyclic compound composed of D-glucopyranose units connected head-to-tail through α-1,4 glycosidic bonds. There are 7 glucose units with an inner diameter of 0.78nm. The structure is as follows: figur...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B37/16G01N24/08C09D105/16
CPCC08B37/0012C09D105/16G01N24/08
Inventor 付强高建勋肖贺廷王丽颖
Owner PTG ADVANCED CATALYST CO LTD
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