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Postprocessing method for glycal reaction solution

A technology of reaction solution and alkenose is applied in the field of post-processing of alkenose reaction solution to achieve the effects of cost saving, high yield and high purity

Active Publication Date: 2012-10-03
SHENGQUAN HEALTANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problems of long working hours, large amount of eluent, low yield and low purity in the post-treatment of the above vinyl sugars, the invention provides a Time-saving, labor-saving, cost-saving and post-processing method of the sugar reaction liquid that can improve the purity and yield of the obtained product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1: Preparation of vinyl sugar reaction solution under anhydrous environment

[0027] Preparation of alkenyl sugar reaction solution: add a mixed solvent of butanone and ethyl acetate to a 5L flask, the volume ratio of butanone and ethyl acetate is 1:1, add 1.5 mol of reducing agent zinc powder, and stir evenly to obtain mixture a; Dissolve 1 mol of 2,3,4-tri-O-acetyl-1-bromo-L-arabinose in a mixed solvent of methyl ethyl ketone and ethyl acetate, and stir evenly to obtain mixture b; heat up and heat mixture a in the flask to reflux, The reflux temperature was 80°C, and the mixture b was added in 10 batches under reflux to obtain the product 3,4-di-O-acetyl-L-arabinose reaction liquid.

[0028] Post-treatment of the sugar reaction solution: after filtering the reaction solution, wash the reaction solution of the sugar reaction solution with a hydrogen ion concentration of 1.14mol / L and a temperature of 2°C until the pH of the water phase is 6, and the treatm...

Embodiment 2

[0032] Embodiment 2: Preparation of vinyl sugar reaction solution under water environment

[0033] Preparation of sugar reaction liquid: add 4L water to a 10L flask, add 8mol sodium bicarbonate white powder to dissolve, then add 10mol zinc powder, 72g copper sulfate pentahydrate solid dissolve, add 1mol tetra-O-acetyl-1-bromo Substitute-D-galactose, and react at room temperature for 24 hours to obtain the product tri-O-acetyl-D-galactenose reaction solution.

[0034] Post-treatment of the sugar reaction solution: after filtering the reaction solution, wash the reaction solution with a dilute sulfuric acid solution with a hydrogen ion concentration of 2.85 mol / L and a temperature of 10°C until the pH of the aqueous phase is 5, and the treatment time is 20 minutes; phase separation, The organic phase is then washed with 20% sodium carbonate solution until the pH of the aqueous phase is 12; the phases are separated, the organic phase is washed with water until the pH of the aqu...

Embodiment 3

[0041] Add dichloromethane to a 5L flask, add 1.5mol reducing agent zinc powder, stir well to obtain mixture a; use dichloromethane to dissolve 1mol tetra-O-acetyl-1-bromo-D-glucose, stir uniformly to obtain mixture b; heat up and heat the mixture a in the flask to reflux, the reflux temperature is 40 degrees, and add the mixture b to it in 10 batches under the reflux state to obtain the product tri-O-acetyl-D-glucal reaction liquid.

[0042] Post-treatment of the sugar reaction liquid: after filtering the reaction liquid, wash the reaction liquid with dilute hydrochloric acid with a hydrogen ion concentration of 2mol / L and a temperature of 5°C until the pH of the aqueous phase is 6.5, and the treatment time is 10 minutes; phase separation , the organic phase was washed with water until the pH of the aqueous phase was 7.2; the phases were separated, and the organic phase was dried and concentrated to obtain 0.935 mol of the product with a detection purity of 94.6%.

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Abstract

The invention relates to the technical field of glycal, in particular to a postprocessing method for a glycal reaction solution. The glycal reaction solution is washed with acid within one hour until the aqueous phase PH is acidic or neutral, then the glycal reaction solution is washed until the aqueous phase PH is neutral or alkaline, organic phases are separated, and the purified glycal is obtained after drying. According to the postprocessing method for the glycal reaction solution disclosed by the invention, time, labor and cost are saved, waste eluent which can not be processed can not be largely produced, the yield and the purity of the obtained glycal are high, and the method can be used for production on a large scale.

Description

[0001] technical field [0002] The invention relates to the technical field of vinyl sugars, in particular to a method for post-processing a vinyl sugar reaction liquid. [0003] Background technique [0004] Sugar compounds are indispensable substances for people's life and production activities. At the same time, sugar also plays a key role in the process of life. Together with nucleic acid and protein, sugar is called the three major living substances. In recent years, with the development of glycobiology and people's high attention to sugar drugs, glycochemistry has entered a period of rapid development, and more and more chemists and research groups at home and abroad have devoted themselves to the research of glycochemistry. At present, the use and sales of sugar drugs have occupied a large proportion in the drug market. According to statistics, there are about 500 kinds of carbohydrate drugs currently on the market. Since most carbohydrate drugs act on the cell sur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H13/06C07H1/06
Inventor 唐地源刘顶王恩华
Owner SHENGQUAN HEALTANG
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