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Method for improving yield and purity of dibromodulcitol substitution reaction product

A technology of dibromodunglitol and reaction products, which is applied in the field of chemical medicine, can solve problems such as dangerous operation process and complex process, and achieve the effect of low equipment requirements, high purity, and easy control

Active Publication Date: 2016-07-27
GUANGXI WUZHOU PHARMA GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The highest concentration of hydrobromic acid that can be purchased in the market is 62%. If it exceeds this concentration, it must be prepared by itself. The process is complicated, the operation process is very dangerous, and the preparation may not be successful.

Method used

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  • Method for improving yield and purity of dibromodulcitol substitution reaction product
  • Method for improving yield and purity of dibromodulcitol substitution reaction product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1: prepare hydrobromic acid acetic acid solution

[0028] At a temperature lower than -5°C, inject hydrogen bromide gas into acetic acid with a concentration of 60-100% to obtain a hydrobromic acid solution with a concentration of 30%.

Embodiment 2

[0029] Embodiment 2: prepare hydrobromic acid acetic acid solution

[0030] At a temperature lower than -10°C, inject hydrogen bromide gas into acetic acid with a concentration of 60-100% to obtain a hydrobromic acid solution with a concentration of 60%.

Embodiment 3

[0032] 1) Get 5.0kg of dulcitol in the reaction kettle, add 1 times the weight of dulcitol, and a hydrobromic acetic acid solution with a concentration of 30%, at the same time, add perchloric acid by 0.5% of the quality of dulcitol, and seal the reaction vessel , feed hydrogen bromide gas, keep the pressure at 0.2Mpa, keep the temperature at 30°C, and keep stirring for 10 hours.

[0033] 2) Add purified water with 10 times the weight of dulcitol and stir for 2 hours. After standing for 12 hours, remove the supernatant, then add 0.1 times the weight of dulcitol and ethanol with a concentration of 70%, stir evenly, filter, and filter the residue with purified After washing with water to neutrality, wash with 70% ethanol at a concentration of 1 times the weight of dulcitol, and dry the collected solid at 27° C. for 36 hours to obtain dibromodulcitol.

[0034] Experimental results: The average yield of dibromodunglitol is 51.0%, and the average purity is 82.2%.

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Abstract

The invention relates to a method for improving yield and purity of a dibromodulcitol substitution reaction product. The method for improving yield and purity of the dibromodulcitol substitution reaction product is used, and the reaction product whose average yield is 50% or above and average purity is 80% or above is obtained; and compared with the prior art, the effect is obviously better.

Description

technical field [0001] The invention relates to the field of chemical medicines, in particular to a method for improving the yield and purity of dibromodunglitol substitution reaction products. Background technique [0002] Dibromogalactitol, also known as dibromogalactitol, is an isomer of dibromomannitol. Although it is generally considered to be an alkylating agent, its effect cannot be fully explained by the alkylation theory, and its inhibition on DNA synthesis is relatively high. RNA synthesis inhibition is strong, and its main metabolite in the body is bis-epoxide, which is a non-specific drug for cell cycle. The LD50 of rats is: oral administration 1400mg / kg, intraperitoneal injection 470mg / kg. The effect is similar to that of dibromomannitol, after being transformed into dehydrodungitol with diethylene oxide structure in the body, it plays an alkylation role. [0003] About the synthesis of dibromodunglitol, following preparation method has been disclosed: [000...

Claims

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Application Information

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IPC IPC(8): C07C31/42C07C29/62
Inventor 许淑清陈明刘冠萍赖树生张栩颜
Owner GUANGXI WUZHOU PHARMA GRP