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Synthetic method for hydroxypropyl-beta-cyclodextrin

A synthesis method and technology of cyclodextrin, which is applied in the field of dextrin etherification, can solve the problems of long reaction time and cumbersome operation, and achieve the effects of short etherification time, simple process and low impurity content

Inactive Publication Date: 2009-09-02
NANJING WELL CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The etherification reaction of the above synthesis method is carried out under open and normal pressure, and the propylene oxide needs to be slowly added dropwise at low temperature, which is cumbersome to operate, and the reaction time is long, generally more than 20 hours, and there are potential safety hazards

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Add 15g of sodium hydroxide and 250ml of deionized water into a 2L stainless steel autoclave, stir to dissolve, weigh 200g of β-cyclodextrin into the autoclave, seal the autoclave, stir, vacuumize, N 2 Replace the gas twice, start to raise the temperature, and stir at 80°C for 1 hour to fully dissolve the β-cyclodextrin. Pass 64g of propylene oxide into the autoclave in 3 batches. Stir the reaction at ℃ for 4 hours. After the reaction, cool down, discharge, neutralize, filter, wash with ethanol, extract with acetone, dialysis and other post-treatments to obtain 151.4 g of hydroxypropyl-β-cyclodextrin, with a yield of 75.7 %, see attached table 1 for product quality indicators.

Embodiment 2

[0037] Add 15g of sodium hydroxide and 250ml of deionized water into a 2L stainless steel autoclave, stir to dissolve, weigh 200g of β-cyclodextrin into the autoclave, seal the autoclave, stir, vacuumize, N 2 Replace the gas twice, start to raise the temperature, and stir at 80°C for 1 hour to fully dissolve the β-cyclodextrin. Pass 64g of propylene oxide into the autoclave in 3 batches. Stir and react at ℃ for 3 hours. After the reaction, cool down, discharge, neutralize, filter, wash with ethanol, extract with acetone, dialysis and other post-treatments to obtain 150.2 g of hydroxypropyl-β-cyclodextrin, with a yield of 75.1 %, see attached table 1 for product quality indicators.

Embodiment 3

[0039] Add 15g of sodium hydroxide and 250ml of deionized water into a 2L stainless steel autoclave, stir to dissolve, weigh 200g of β-cyclodextrin into the autoclave, seal the autoclave, stir, vacuumize, and replace with N2 gas twice, Start to heat up, stir at 80°C for 1 hour to fully dissolve the β-cyclodextrin, pass 82g of propylene oxide into the autoclave in 3 batches, after the completion, stir and react at 0.2MPa and 80°C for 4 hours, After the reaction, cool down, discharge, neutralize, filter, wash with ethanol, extract with acetone, dialysis and other post-treatments to obtain 160.2g of hydroxypropyl-β-cyclodextrin with a yield of 80.1%. Table 1.

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Abstract

The invention relates to a synthetic method for hydroxypropyl-beta-cyclodextrin. The synthetic method is characterized by comprising the following steps: (1) charging beta-cyclodextrin, propylene oxide, basic catalyst and deionized water in a molar ratio of 1:2.5-10.5:0.6-3.4:62.9-126 into a closed stainless steel high-pressure autoclave, and carrying out etherification reaction on the materials at a temperature of between 50 and 90 DEG C and a gauge pressure of between 0 and 0.6MPa; (2) neutralizing and filtering the mixture after the reaction; (3) washing the mixture with ethanol; (4) extracting with acetone; and (5) obtaining the hydroxypropyl-beta-cyclodextrin after dialysis and other processes. The synthetic method for the hydroxypropyl-beta-cyclodextrin has higher product yield which can be more than 70 percent (calculated by inventory rating of the beta-cyclodextrin), and the obtained product quality index is in accordance with the 5.0 quality standard of European pharmacopoeia. The synthetic method has the characteristics of simple process, short etherification reaction time, moderate reaction conditions, low impurity content, and the like.

Description

technical field [0001] The invention relates to a method for synthesizing hydroxypropyl-β-cyclodextrin, which belongs to the technical field of dextrin etherification. Background technique [0002] Cyclodextrin (Cyclodextrin.CD) is a natural product of cyclic oligosaccharides formed by linking 6 to 15 glucose molecules obtained from starch through the action of biological enzymes. The common ones are α, β, and γ-cyclodextrin, among which The β-cyclodextrin molecule is in the shape of a circular cylinder with a hollow cavity, and its cavity can contain a large number of other substances to form nano-scale inclusion complexes. The inclusion of β-cyclodextrin can protect the guest molecules in its cylindrical cavity, so it has anti-oxidation, light resistance, heat resistance, slow release, solubilization and other properties; used in medicine, it is also It increases drug stability, promotes absorption, and improves bioavailability; however, the solubility of β-cyclodextrin i...

Claims

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Application Information

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IPC IPC(8): C08B37/16
Inventor 李清华沈德渊贾建国吴仰波高正松
Owner NANJING WELL CHEM
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