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Method for preparing DHBE (dihydroxy dibutyl ether)

A technology of dihydroxydibutyl ether and butanediol is applied in the fields of ether preparation, dehydration of hydroxyl-containing compounds to prepare ether, organic chemistry, etc. Simple processing, low production cost, and the effect of ensuring product quality

Inactive Publication Date: 2013-10-02
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] At present, dihydroxy dibutyl ether mainly uses sulfuric acid catalyst in the industrial production process. Although its technology is mature, in the later separation and purification process, the environmental burden is large, and there are also unavoidable shortcomings, such as difficult recovery of the catalyst, Corrosion-prone equipment, difficulty in continuous production, low yield, high water and energy consumption, and difficult treatment of sulfuric acid waste liquid, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Measure 150.0g (0.83mol) of 1,3-butanediol into a well-sealed 250ml three-necked bottle equipped with a thermometer, add 1% composite metal oxide solid super acid together, stir, heat in an oil bath, and After reaching the reaction temperature of 185-190°C, the reaction was carried out for 4 hours, and the conversion rate was 57%. After the product was cooled to room temperature, the solid superacid catalyst was removed by filtration, and the product was distilled under reduced pressure (114-124°C / 5mm Hg) to obtain dihydroxydibutyl ether. Measured by GC, the product content is 96.1%.

Embodiment 2

[0028] Measure 150.0g (0.83mol) of 1,3-butanediol into a three-necked flask, add 5% composite metal oxide solid superacid together, stir, heat in an oil bath, and rise to a reaction temperature of 115-152°C, After 1.5 hours of reaction, the conversion rate was 82%. After the product was cooled to room temperature, the product was distilled under reduced pressure (114-124°C / 5mm Hg) to obtain dihydroxydibutyl ether. As determined by GC, the product content is 97.8%.

Embodiment 3

[0030] Measure 150.0g (0.83mol) of 1,3-butanediol into a three-necked flask, add 15% composite metal oxide solid super acid together, stir, heat in an oil bath, and rise to a reaction temperature of 117-148°C, After 1 hour of reaction, the conversion rate was 80%. After the product is cooled to room temperature, the product is distilled under reduced pressure to obtain a dihydroxy dibutyl ether product. As determined by GC, the product content is 95.3%.

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Abstract

The invention relates to the field of chemical material preparation and discloses an efficient and simple method for preparing DHBE (dihydroxy dibutyl ether) for drug use. The method comprises the following steps of catalyzing 1,3-butanediol with a solid superacid catalyst with mass percentage of 1.0%-50% or a hydrogen molecular sieve based catalyst at 50-190 DEG C so as to prepare the dihydroxy dibutyl ether through condensation, after reaction, cooling and filtering the product, and obtaining the dihydroxy dibutyl ether with content more than or equal to 95 percent through reduced pressure distillation of the product. The dihydroxy dibutyl ether is suitable for being used as bulk drug of cholagogue Dyskinebul, and the method is environment-friendly and efficient, has low cost, is simple to operate, and is suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of chemical raw material preparation, in particular to a green preparation method of dihydroxy dibutyl ether. The product can be used as an auxiliary drug for hepatobiliary diseases. Background technique [0002] Dihydroxydibutyl ether (dihudroxudibutylether, DHBE) is a colorless, odorless, light yellow oily liquid, which is widely used in fine chemical fields such as pharmaceuticals, industrial detergents and dispersants. Especially in the field of medicine, dihydroxydibutyl ether (DHBE) capsules have been marketed as a drug for the treatment of liver and gallbladder diseases and have been listed in many countries. The trade name is Dyskinebul (Dyskinebul), which was first successfully developed and put on the market by the French Laphal pharmaceutical company. The drug belongs to bile secretion bidirectional enhancer, has functions of promoting choleresis, anti-inflammation, relieving spasm, protecting gallbladder...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/13C07C41/09
Inventor 孟庆伟朱晓桐都健姚鸿杰刘广志李智
Owner DALIAN UNIV OF TECH
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