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Method for preparing dianhydrogalactitol

A kind of technology of dulcitol dihydrate and dulcitol dibromo, applied in directions such as organic chemistry, drug combination, antitumor drugs, etc., can solve problems such as high preparation cost, narrow source of raw materials, etc., achieve the reduction of miscellaneous peaks, reduce production The effect of improving cost and purity

Inactive Publication Date: 2014-07-16
天津中津药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has narrow sources of raw materials and high preparation costs

Method used

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  • Method for preparing dianhydrogalactitol
  • Method for preparing dianhydrogalactitol
  • Method for preparing dianhydrogalactitol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Wash and crush the corn cob to 1mm, add deionized water according to the ratio of material to water 1:3, heat to 100°C, keep warm and stir for 2 hours; after filtering, add 5 times the volume of corn cob to the solid, with a mass concentration of 5% Hydrochloric acid, at room temperature, 100 MHz ultrasonic treatment for 1.5 hours, heated to 100 ° C for hydrolysis, refluxed for 2 hours, and suction filtered to obtain the hydrolyzate. The hydrolyzate still contains HCl, so it needs to be neutralized. Heat the above hydrolyzate to 78°C, add calcium carbonate emulsion with a specific gravity of 0.9 while stirring, and adjust the pH to 7. In order to make the precipitation fully, keep it warm for 1 hour after neutralization, and filter to remove the residue. Evaporate the sugar liquid after deslagging under reduced pressure, and the obtained material liquid is xylose mother liquor. It has been detected that the feed liquid contains galactose.

[0036] Take the xylose moth...

Embodiment 2

[0041] Wash and crush the bagasse to 2mm, add deionized water according to the ratio of material to water 1:3, heat to 100°C, keep stirring for 3 hours; after filtering, add 5 times the volume of solid to the solid, hydrochloric acid with a mass concentration of 5%, at room temperature , frequency 100MHz ultrasonic treatment for 2 hours, heated up to 100°C for hydrolysis, refluxed for 1 hour, and suction filtered to obtain the hydrolyzate. Heat the above hydrolyzate to 80°C, add calcium carbonate emulsion with a specific gravity of 1.05 while stirring, and adjust the pH to 6.5. In order to make the precipitation fully, keep it warm for 1 hour after neutralization, and filter to remove the residue. Evaporate the sugar liquid after deslagging under reduced pressure, and the obtained material liquid is xylose mother liquor. It has been detected that the feed liquid contains galactose.

[0042] Take the xylose mother liquor whose mass concentration is 65%, add deionized water to ...

Embodiment 3

[0046] Wash and grind the corn cob and bagasse to 1mm, add deionized water according to the ratio of material to water 1:3, heat to 80°C, keep stirring for 4 hours; add 5 times the volume of solids, hydrochloric acid with a mass concentration of 3% after draining, and store at room temperature , frequency 100MHz ultrasonic treatment for 1.5 hours, heated up to 100°C for hydrolysis, refluxed for 1.5 hours, and suction filtered to obtain the hydrolyzate. Heat the above hydrolyzed solution to 78°C, add calcium carbonate emulsion with a specific gravity of 0.9 while stirring, adjust the pH to 7, in order to fully precipitate, keep warm for 1.5 hours after neutralization, and filter to remove residue. Evaporate the sugar liquid after deslagging under reduced pressure, and the obtained material liquid is xylose mother liquor. It has been detected that the feed liquid contains galactose.

[0047] Take the xylose mother liquor whose mass concentration is 65%, add deionized water to d...

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Abstract

The invention discloses a method for preparing dianhydrogalactitol. The method comprises the following steps: diluting by a xylose mother liquor, carrying out decoloring filtration, carrying out ion exchange, and carrying out chromatographic separation to obtain a xylose and glucose mixed liquor and a galactose and arabinose mixed liquor; carrying out evaporative concentration on the galactose and arabinose mixed liquor, carrying out catalytic hydrogenation, carrying out decoloring filtration, carrying out ion exchange, and evaporating to supersaturation in order to obtain crystallized dulcitol; and reacting dulcitol with hydrobromic acid to prepare 1,6-bromodulcitol; and dissolving 1,6-bromodulcitol in t-butyl alcohol of potash, and carrying out an elimination reaction to prepare dianhydrogalactitol. The xylose mother liquor can be prepared by hydrolyzing one or more of corncobs, bagasse, sugarcane pith, cottonseed hulls and rice hulls. Highly pure dianhydrogalactitol can be produced through the method.

Description

【Technical field】 [0001] The invention relates to a preparation method, in particular to a method for preparing dianhydrodulcitol. 【Background technique】 [0002] Xylitol, also known as pentapentyl alcohol, is a five-carbon sugar alcohol with a molecular formula of C 5 h 12 o 5 , is an intermediate product of xylose metabolism, widely present in foods such as fruits, vegetables, cereals, mushrooms, and plants such as wood, straw, and corn cobs. As a sweetener, xylitol is widely used in the food industry, and as a clinical nutritional and therapeutic agent for patients with diabetes and hepatitis. In addition, it is an important chemical raw material, widely used in leather, plastics and coatings. Dulcitol, also known as sweet alcohol, galactitol, hexyl alcohol, the molecular formula is C 6 h 14 o 6 . In nature, it mainly exists in some plants of the genus Osmanthus and chervil. Because its content is very low and it is often mixed with other substances, the productio...

Claims

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Application Information

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IPC IPC(8): C07D303/14C07D301/26A61P35/00
CPCC07D301/26C07D303/14
Inventor 宋富智李德山梁世昌宋德顺
Owner 天津中津药业股份有限公司
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