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Refining method of hydrochloric acid ambroxol compound

A kind of technology of ambroxol hydrochloride and crude product of ambroxol hydrochloride, which is applied in the field of ambroxol hydrochloride compound and its preparation method, can solve the problems such as the content reduction of the active ingredient of the drug, the purity of the drug does not meet the requirements, and the improper control of the production process. Improving respiratory conditions, simple and easy refining process, and improving the effect of clinical adverse reactions

Active Publication Date: 2013-09-25
灵康药业集团股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In addition, when the compound is improperly stored or stored for a long time, the content of the active ingredient of the drug will decrease, the color will increase, and the content of related substances will increase.
In some cases, the purity of the drug did not meet the requirements due to improper control of the manufacturing process
The prior art does not disclose a special purification method for this, so it is necessary to further purify such unqualified products or crude products, and refine them into high-purity compounds with high yields

Method used

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  • Refining method of hydrochloric acid ambroxol compound

Examples

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Comparison scheme
Effect test

Embodiment 1

[0048] The refining of embodiment 1 ambroxol hydrochloride

[0049] The ambroxol hydrochloride crude product (its HPLC purity is 92.52%) that 10g is made according to prior art method is dissolved in 80ml methanol, stirs, makes it dissolve completely, then adds the gac of 0.3g, stirs and adsorbs for 20 minutes, filters and removes charcoal, collect the filtrate; add 10g aluminum oxide after concentration and stir evenly, add to the upper end of the preparative chromatographic column after the solvent is evaporated, and then use the preparative chromatographic column to separate and purify the filtrate, wherein the mobile phase used in the chromatographic column is a volume ratio of 1:1.5 mixed solvent of acetonitrile and water, the flow rate is 0.2ml / min, the stationary phase filler is ICN allumina N neutral alumina with a particle diameter of 18-32 μm and a pore diameter of 6nm, the column temperature is room temperature, and the wavelength is 248nm. Deliquified, concentrat...

Embodiment 2

[0059] The refining of embodiment 2 ambroxol hydrochloride

[0060] 10g ambroxol hydrochloride crude drug (pharmaceutical factory: Shandong Luoxin Pharmaceutical Co., Ltd., lot number: 20091102; HPLC purity is 92.76%) is dissolved in 100ml ethanol under heating, stirs, and it is dissolved completely, then adds 0.2 g of activated carbon, stirred and adsorbed for 15 minutes, filtered for decarbonization, and collected the filtrate; after concentrating, add 10 g of alumina and stir evenly, evaporate the solvent and add it to the upper end of the preparative chromatographic column, and then use the preparative chromatographic column to separate and purify the filtrate. Wherein the mobile phase used in the chromatographic column is a mixed solvent of methanol and water with a volume ratio of 1:1.2, the flow rate is 2ml / min, and the stationary phase filler is a Baker column chromatography special neutral alumina with a particle size of 50-200 μm and a pore size of 6 nm. The column...

Embodiment 3

[0065] The refining of embodiment 3 ambroxol hydrochloride

[0066] 10g ambroxol hydrochloride bulk drug (pharmaceutical factory: Shandong Luoxin Pharmaceutical Co., Ltd., batch number: 20091102; HPLC purity is 92.76%) is dissolved in 120ml ethylene glycol under heating, stirs, and it is dissolved completely, then Add 0.4g of activated carbon, stir and adsorb for 15 minutes, filter and decarbonize, and collect the filtrate; after concentration, add 15g of alumina and stir evenly, evaporate the solvent and add to the upper end of the preparative chromatographic column, and then separate and purify the filtrate. The mobile phase used is a mixed solvent of methanol and water with a volume ratio of 1:1.8, the flow rate is 1ml / min, the stationary phase filler is ICN allumina N neutral alumina with a particle size of 18-32 μm and a pore size of 6 nm, and the column temperature is Room temperature, wavelength 248nm, collect the eluate, and concentrate under reduced pressure at 50°C. ...

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Abstract

The invention relates to a hydrochloric acid ambroxol compound and a novel preparation method thereof, which include the following steps: 1, dissolving coarse hydrochloric acid ambroxol with certain amount into solvent, adding active carbon for adsorption, filtering, collecting filtering liquid and conducting decompressing and concentration; 2 conducting separation purification on concentration liquid through a preparation type chromatographic column, collecting eluent and conducting decompressing and concentration; and 3 conducting negative pressure crystallization on hydrochloric acid ambroxol concentration liquid obtained in the step2, first conducting concentration under negative pressure and rising temperature, then reducing temperature, adding hydrochloric acid ambroxol seed crystal, maintaining the temperature till the ideal crystal is obtained if fine crystal occurs, separating the precipitated crystal by filtering or centrifugation and conducting washing and drying on the crystal to finally obtain purified hydrochloric acid ambroxol. The hydrochloric acid ambroxol prepared in the method is high in purity, even in crystal, complete in crystal shape, good in flowing performance and large in processing quantity. The reaction can be conducted continuously, so that the method is especially suitable for industrial production. Simultaneously, the hydrochloric acid ambroxol compound and the method improve product quality and reduce toxic side effect.

Description

technical field [0001] The invention relates to an ambroxol hydrochloride compound and a preparation method thereof, belonging to the technical field of medicine. Background technique [0002] Ambroxol hydrochloride (Ornidazole), white to slightly yellow crystalline powder; almost odorless, chemical name: trans-4-[(2-amino3.5-dibromobenzyl)amino]cyclohexanol hydrochloride, molecular formula: C 13 h 18 Br 2 N 2 O HCl, molecular weight: 414.57, structural formula: [0003] [0004] Ambroxol hydrochloride has the characteristics of promoting mucus elimination and dissolving secretions. It can promote the elimination of viscous secretions in the respiratory tract and reduce the retention of mucus, thus significantly promoting expectoration and improving respiratory conditions. When this product is used for treatment, the patient's mucus secretion can return to normal conditions. Cough and sputum volume are usually significantly reduced, and the surfactant on the respira...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C215/44C07C213/10
Inventor 陶灵刚曹丽梅吕强张凤廖爱国李双喜
Owner 灵康药业集团股份有限公司
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