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Green preparation method of dihydroxy dibutyl ether

A green technology of dihydroxy dibutyl ether, which is applied in the field of green preparation of dihydroxy dibutyl ether, can solve the problems of easy-to-corrosion equipment, low yield, high water consumption and energy consumption, etc., to ensure product quality, simple treatment, The effect of low production cost

Active Publication Date: 2013-09-25
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% polystyrene sulfonic acid resin catalyst together, stir, heat in an oil bath, and After reaching the reaction temperature of 165-170°C, the reaction was carried out for 4 hours, and the conversion rate was 57%. After the product was cooled to room temperature, the sulfonic acid resin catalyst was removed by filtration, and the product was distilled under reduced pressure (114-124°C / 5mm Hg) to obtain dihydroxydibutyl ether. , determined by GC, the product content is 95.5%.

Embodiment 2

[0028] Measure 150.0g (0.83mol) of 1,3-butanediol into a three-necked flask, add 18% polystyrene sulfonic acid resin catalyst together, stir, heat in an oil bath, and rise to a reaction temperature of 135-152°C, After 1.3 hours of reaction, the conversion rate was 72%. After the product was cooled to room temperature, the product was distilled under reduced pressure (114-124°C / 5mm Hg) to obtain dihydroxydibutyl ether. Measured by GC, the product content is 96.3%.

Embodiment 3

[0030] Measure 150.0g (0.83mol) of 1,3-butanediol into a three-necked flask, add 10% polystyrene sulfonic acid resin catalyst together, stir, heat in an oil bath, and rise to a reaction temperature of 137-148°C, After 1.8 hours of reaction, the conversion rate was 68%. After the product was cooled to room temperature, the product was distilled under reduced pressure to obtain the dihydroxy dibutyl ether product. The product content was 96.6% as determined by GC.

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Abstract

The invention relates to the field of preparation of chemical raw materials, and discloses a high-efficiency simple method for preparing dihydroxy dibutyl ether which satisfies the medicinal standard. The method comprises the following steps: condensing 1,3-butanediol at 70-190 DEG C by using 1.0-80 wt% cation exchange resin catalyst as a cation exchange resin catalyst to prepare dihydroxy dibutyl ether; and after the reaction finishes, cooling the reaction solution, filtering, and distilling under reduced pressure to obtain the dihydroxy dibutyl ether of which the content is at least 97%. The product is suitable for producing an active pharmaceutical ingredient of cholagogue Baodanjiansu. The method has the advantages of environmental protection, high efficiency and low cost, and is simple to operate and suitable for industrial large-scale 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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IPC IPC(8): C07C43/13C07C41/09
Inventor 孟庆伟朱晓桐姚鸿杰刘广志李智都健
Owner DALIAN UNIV OF TECH
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