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New green synthesis technology of ethylated-beta-cyclodextrin

A technology for green synthesis and cyclodextrin, applied in the field of synthesis technology of ethylated-β-cyclodextrin, can solve problems such as limited application, and achieve the effects of high conversion rate, simple process conditions and environmental friendliness

Inactive Publication Date: 2014-03-19
FUJIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Bromoethane (or iodoethane) and diethyl sulfate are toxic reagents, which limit the application of ethylated-β-cyclodextrin

Method used

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  • New green synthesis technology of ethylated-beta-cyclodextrin
  • New green synthesis technology of ethylated-beta-cyclodextrin

Examples

Experimental program
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Effect test

Embodiment 1

[0020] In a three-necked round-bottomed flask with a reflux condenser and stirring, add 2 g of β-cyclodextrin (1.8 mmol) and 150 mL of DMF (dimethylformamide) and stir until clear, then add 1.0 g of K 2 CO 3 , stirred for 10 minutes, then added 4.0mL (63mmol) diethyl carbonate, continued to stir, heated in an oil bath to control the temperature at 125°C, and reacted for 24 hours. During the entire reaction process, a protective gas was introduced, and the reaction process was performed by thin-layer chromatography ( TLC) to monitor the reaction. After the reaction, K was removed by centrifugation 2 CO 3 and suspended matter, under reduced pressure, the liquid phase temperature is 60-115°C, the solvent DMF and unreacted diethyl carbonate are distilled off under reduced pressure, the solution is concentrated with DMF less than 5% (mass percentage), and 100mL of acetone is added to it after cooling, Stir, filter off the acetone, soak the obtained solid powder in anhydrous ethe...

Embodiment 2

[0025] In a three-necked round bottom flask with a reflux condenser and stirring, add 2g β-cyclodextrin (1.8mmol) and 90mL DMF and stir until clear, then add 1.0g K2CO3, stir for 10 minutes and then add 3.0mL (46mmol ) diethyl carbonate, continue to stir, heat in an oil bath to control the temperature at 110°C, and react for 24 hours. During the entire reaction process, a protective gas must be introduced, and the reaction process is monitored by thin layer chromatography (TLC). After the reaction is over, centrifuge to remove Na2CO3 and suspended matter, depressurize, the liquid phase temperature is 60-115°C, distill off the solvent DMF and unreacted diethyl carbonate under reduced pressure, concentrate the solution until the mass percentage of DMF is less than 5%, and cool Then add 100mL of acetone to it, stir, and filter off the acetone. The obtained powder solid is soaked in anhydrous ether for 16 hours, soaked 3 times to obtain 1.83 g of the product, the yield of β-cyclode...

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Abstract

The invention discloses a new green synthesis technology of ethylated-beta-cyclodextrin. The technology comprises the following steps: 1, reacting beta-cyclodextrin with diethyl carbonate in a DMF solvent in the presence of K2CO3 or Na2CO3 at 60-135DEG C for 0.5-56h, and introducing a protection gas in the whole reaction process; 2, filtering for removing K2CO3 or Na2CO3 and other insolubles, carrying out reduced pressure distillation to remove the solvent DMF, and carrying out solution concentration of the mass content of DMF of below 5%; and 3, adding acetone, stirring, precipitating a product, filtering out acetone, immersing the obtained powdery solid in anhydrous ether for 16-24h, and drying to obtain the final product. The technology has the advantages of simple condition, high conversion rate of beta-cyclodextrin, and realization of the conversion rate of beta-cyclodextrin after the reaction reaching 30-95%, realization of the average degree of substitution of the product reaching1.6-6.5, and environmental protection.

Description

technical field [0001] The invention relates to a synthesis process of ethylated-β-cyclodextrin, in particular to a method of using green ethylating reagent diethyl carbonate to replace diethyl sulfate or ethyl halide, which are toxic to human body and risky to the environment, etc. Ethylating reagent, the process of synthesizing green ethylated-β-cyclodextrin by using diethyl carbonate and β-cyclodextrin. Background technique [0002] β-cyclodextrin has a cavity molecular structure and the characteristics of internal hydrophobicity and external hydrophilicity, and can be widely used in separation, medicine, catalysis, etc.; however, due to the low solubility of β-cyclodextrin parent and inclusion properties limitations, so that its application is limited. In order to extend the physical and chemical properties of β-cyclodextrin, scholars at home and abroad have introduced new groups on the hydroxyl group of β-cyclodextrin, most of which are to increase the solubility of β-...

Claims

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Application Information

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IPC IPC(8): C08B37/16
Inventor 甘永江
Owner FUJIAN UNIV OF TECH
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