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Dihydroxy dibutyl ether synthesized through catalysis with dry hydrogen resin and preparation method of dihydroxy dibutyl ether

A technology of dihydroxydibutyl ether and hydroxydibutyl ether, applied in the field of preparation of dihydroxydibutyl ether, to achieve the effects of overcoming low catalytic activity, avoiding corrosion, and simple operation

Active Publication Date: 2017-10-20
河北凯盛医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the reaction of catalyzing alcohol condensation into ether with NKC-9 resin has not been reported.

Method used

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  • Dihydroxy dibutyl ether synthesized through catalysis with dry hydrogen resin and preparation method of dihydroxy dibutyl ether
  • Dihydroxy dibutyl ether synthesized through catalysis with dry hydrogen resin and preparation method of dihydroxy dibutyl ether
  • Dihydroxy dibutyl ether synthesized through catalysis with dry hydrogen resin and preparation method of dihydroxy dibutyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 30ml of 1,3-butanediol and 0.6g of vacuum-dried NKC-9 macroporous strongly acidic cation exchange resin into a 100ml four-neck flask, heat and stir, and react under reflux for 9 hours. After cooling, the resin was removed by filtration, and the resin was reserved for reuse next time. 5.68 grams of dihydroxydibutyl ether were contained in the mixture recorded by GC.

Embodiment 2

[0024] Add 30ml of 1,3-butanediol and 1.5g of vacuum-dried NKC-9 macroporous strongly acidic cation exchange resin into a 100ml four-neck flask, heat and stir, and react under reflux for 9 hours. After cooling, the resin was removed by filtration, and the resin was reserved for reuse next time, and 6.85 grams of dihydroxydibutyl ether was contained in the mixture recorded by GC.

Embodiment 3

[0026] Add 30ml of 1,3-butanediol and 1.5g of vacuum-dried NKC-9 macroporous strongly acidic cation exchange resin into a 100ml four-neck flask, heat and stir, and react under reflux for 6 hours. After cooling, the resin was removed by filtration, and the resin was reserved for reuse next time, and 5.32 grams of dihydroxydibutyl ether was contained in the mixture recorded by GC.

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Abstract

The invention discloses a novel preparation method for synthesizing dihydroxy dibutyl ether through catalysis of 1,3 butanediol with dry hydrogen resin. The dry hydrogen resin is selected from H type cation exchange resin with the water content lower than or equal to 5%, the resin can be used without regeneration, is simple to treat, has higher catalytic efficiency as compared with wet gel resin in the prior art, has high reuse rate, avoids corrosion caused by sulfuric acid to equipment and is an efficient and environment-friendly catalyst. The process synthesis route is simple, has the mild condition and is an environment-friendly synthesis route prone to industrialization.

Description

technical field [0001] The invention relates to a preparation method of dihydroxydibutyl ether, which belongs to the field of chemical drug synthesis. Background technique [0002] Dihydroxydibutylether (dihydroxydibutylether, DHBE), crude drug is produced by Italy LusochimicaS.P.A company, and its soft capsule preparation is produced by French Laphal large pharmaceutical factory, trade name is health-care element (Dyskinebyl), is a kind of hepatobiliary disease medicine. The drug belongs to bile secretion bidirectional enhancer, has functions of choleretic, anti-inflammatory, antispasmodic, liver-protecting, lipid-lowering and calculus-expelling, and is a truly efficient and ideal choleretic. [0003] Dihydroxydibutyl ether is a pharmacologically active mixture, which is composed of three isomers of hydroxy ethers, these three isomers are: 4-(3-hydroxybutoxy) -2-butanol ( Ⅰ ), 3-(3-hydroxybutoxy)-1-butanol ( Ⅱ ), 3-(3-hydroxy-1-methylpropoxy)-1-butanol ( Ⅲ ). Its struct...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/09C07C43/13B01J31/08
CPCC07C41/09C07C43/13B01J31/08
Inventor 赵凯侯建平秦智巧
Owner 河北凯盛医药科技有限公司
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