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High-purity dihydroxybutyl ether and preparation method thereof

A dihydroxydibutyl ether, high-purity technology, applied in ether preparation, dehydration of hydroxyl-containing compounds to prepare ether, ether separation/purification, etc., can solve the problems of strong corrosion of equipment, high production cost, and potential safety hazards, etc. Achieve the effect of good product quality, avoid corrosion, and reduce the pollution of three wastes

Active Publication Date: 2014-06-11
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

[0006] Among the above three methods, the first method uses expensive and highly active sodium hydride, which has high cost and great safety hazards; in addition, the highly toxic reagent dioxane
The second method uses relatively expensive α-methyl-γ-methoxypropanol as a starting material and concentrated sulfuric acid as a catalyst. The former causes high production costs, and the latter is highly corrosive to equipment
In the third method, although cheap 1,3-butanediol is used as a starting material, concentrated sulfuric acid is still used as a catalyst

Method used

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  • High-purity dihydroxybutyl ether and preparation method thereof
  • High-purity dihydroxybutyl ether and preparation method thereof
  • High-purity dihydroxybutyl ether and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Add 300ml of 1,3-butanediol and 40g of pretreated 001×7 type strongly acidic cation exchange resin into a 1000ml four-neck flask, heat and stir, and react to remove water for 4h. After cooling down, remove the resin by filtration, the measured pH of the solution is about 5-6, adjust to neutral with a little NaOH solution. The crude product was obtained by distillation under reduced pressure. After the crude product was washed with petroleum ether and vacuum rectified, the 156~161°C / 20mmHg fraction was collected to obtain 55.4g with a gas phase purity of 98.4%.

Embodiment 2

[0035] Add 300ml of 1,3-butanediol and 60g of pretreated 001×7 type strongly acidic cation exchange resin into a 1000ml four-neck flask, heat and stir, and react to remove water for 3.5h. After cooling down, remove the resin by filtration, measure the pH of the solution to be about 5-6, and adjust it to neutral with a little NaOH solution. The crude product was obtained by distillation under reduced pressure. After the crude product was washed with petroleum ether and vacuum rectified, the 156~161°C / 20mmHg fraction was collected to obtain 58.3g with a gas phase purity of 98.5%.

Embodiment 3

[0037] Add 300ml of 1,3-butanediol and 60g of pretreated 001×7 type strong acid cation exchange resin into a 1000ml four-neck flask, heat and stir, react to remove water for 4 hours, filter and remove the resin after cooling down, and measure the pH of the solution to be about 5~ 6. Adjust to neutral with a little NaOH solution. The crude product was obtained by distillation under reduced pressure. After the crude product was washed with petroleum ether and rectified in vacuum, the 156~161°C / 20mmHg fraction was collected to obtain 59.0g, gas phase pure Degree 98.5% .

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Abstract

The invention discloses a new preparation method of high-purity dihydroxybutyl ether, and the new preparation method comprises the following steps: treating 1,3-butanediolby by using acidic cationic resin, performing reduced pressure distillation to obtain a dihydroxybutyl ethercrude product, treating the crude product by using petroleum ether and then performing vacuum rectification to prepare the high-purity dihydroxybutyl ether. The process route has the advantage of overcoming the corrosion caused by use of sulfuric acid to the equipment and has the characteristics of short reaction steps, gentle condition, simplicity in operation, high yield, high product purity and the like, so that the process route is an environment-friendly synthesis route easy for industrialization.

Description

technical field [0001] The invention relates to a preparation method of dihydroxydibutyl ether (cholebumin) and belongs to the field of chemical drug synthesis. Background technique [0002] Dihydroxydibutylether Soft Capsules, the English name is Dihydroxydibutylether Soft Capsules, and the trade name is Baodanjiansu, which is an adjuvant drug for liver and gallbladder diseases. It was successfully developed and put on the market by the French Laphal Pharmaceutical Company. my country has approved the import of this drug for the treatment of liver and gallbladder diseases. The drug belongs to bile secretion bidirectional enhancer, has functions of choleretic, anti-inflammatory, antispasmodic, liver-protecting, lipid-lowering, stone-expelling, and is a truly efficient and ideal choleretic. [0003] Dihydroxydibutyl ether (Baotanjiansu) is a pharmacologically active mixture composed of several hydroxy ethers that are isomers of each other. It is reported in the literature t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/09C07C43/13
CPCC07C41/09C07C41/34C07C43/132
Inventor 赵凯侯建平赵新颖王伟杰苑洪忠赵亚峰
Owner 河北凯盛医药科技有限公司