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A kind of preparation method of ambroxol hydrochloride impurity standard substance

A technology for ambroxol hydrochloride and a standard product, applied in the field of medicine, can solve problems such as synthesis and content calibration methods that have not been reported, and achieve control of the quality of ambroxol hydrochloride raw materials and preparations thereof, the raw materials are cheap and easy to obtain, and the preparation process is simple and convenient Effect

Active Publication Date: 2018-09-11
HEFEI JIUNUO MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no report on the synthesis and content calibration method of this impurity

Method used

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  • A kind of preparation method of ambroxol hydrochloride impurity standard substance
  • A kind of preparation method of ambroxol hydrochloride impurity standard substance
  • A kind of preparation method of ambroxol hydrochloride impurity standard substance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] The preparation method of ambroxol hydrochloride impurity standard substance in the present embodiment is as follows:

[0046] 1. Disperse 8g (19.28mmol) of ambroxol hydrochloride in 100ml of water, add sodium hydroxide solution to adjust the pH value to 10, then add 200ml of ethyl acetate, extract, wash the extract with water, concentrate the organic phase to obtain an oily liquid, add formic acid 50ml of isopropyl ester, reflux and stir for 6h, stir to cool down to 0-5°C, keep stirring for 3h, filter, and dry the solid at 50-60°C for 4h under reduced pressure to obtain 4-(6,8-dibromo-3,4- Dihydroquinazolin-3-yl)-cyclohexanol crude product 6.9g, yield 92.12%.

[0047] 2. Add 100ml of isopropanol to 6.8g of crude product, heat and stir at 80-100°C to dissolve, filter while hot, cool the filtrate to -5-0°C, stir and crystallize for 4 hours, filter, wash the filter cake with an appropriate amount of isopropanol, The solid was dried under reduced pressure at 50-60°C for 5...

Embodiment 2

[0058] The preparation method of ambroxol hydrochloride impurity standard substance in the present embodiment is as follows:

[0059] 1. Disperse 10 g (24.12 mmol) of ambroxol hydrochloride in 100 ml of water, add sodium carbonate solution to adjust the pH value to 10, then add 200 ml of ethyl acetate, extract, wash the extract with water, concentrate the organic phase to obtain an oily liquid, add formic acid 50ml of butyl ester, stirred and reacted at 100°C for 5h, stirred and cooled to 0-5°C, kept stirring for 4h, filtered, and the solid was dried under reduced pressure at 50-60°C for 5h to obtain 4-(6,8-dibromo-3,4 -Dihydroquinazolin-3-yl)-cyclohexanol crude product 8.6g, yield 91.88%.

[0060] 2. Add 80ml of ethanol to 8g of crude product, heat and stir at 80°C to dissolve, filter while hot, cool the filtrate to -5~0°C, stir and crystallize for 4h, filter, wash the filter cake with an appropriate amount of ethanol, and decompose the solid at 50~60°C Dry under pressure fo...

Embodiment 3

[0065] The preparation method of ambroxol hydrochloride impurity standard substance in the present embodiment is as follows:

[0066] 1. Disperse 12g (28.95mmol) of ambroxol hydrochloride in 100ml of water, add sodium carbonate to adjust the pH to 9, then add 200ml of ethyl acetate, extract, wash the extract with water, concentrate the organic phase to obtain an oily liquid, add n-butyl formate 50ml, stirred and reacted at 100°C for 5h, stirred and cooled to 0-5°C, kept stirring for 5h, filtered, and the solid was dried under reduced pressure at 50-60°C for 6h to obtain 4-(6,8-dibromo-3,4-di Hydroquinazolin-3-yl)-cyclohexanol crude product 10.4g, yield 92.86%.

[0067] 2. Add 110ml of n-butanol to 10g of crude product, heat and stir at 80°C to dissolve, filter while hot, cool the filtrate to -5~0°C, stir and crystallize for 3h, filter, wash the filter cake with an appropriate amount of ethanol, and the solid is at 50~60 After drying under reduced pressure at ℃ for 4 hours, 9....

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Abstract

The invention discloses a preparation method for an impurity standard substance of ambroxol hydrochloride. The method comprises the steps of alkalizing ambroxol hydrochloride, which serves as a raw material, with an inorganic base so as to obtain free ambroxol, condensing ambroxol with formate so as to obtain a crude product, and refining the crude product, thereby obtaining pure 4-(6,8-dibromo-3,4-dihydro quinazolin-3-yl)-cyclohexanol. According to the impurity preparation method provided by the invention, the raw material is cheap and readily available, the process is simple, the preparation cycle is short, and proven by standardization, the product content is higher than 98.5%. The ambroxol hydrochloride impurity provided by the invention can be applied to the qualitative and quantitative research and detection on impurities of the ambroxol hydrochloride raw material and preparations thereof as the impurity standard substance.

Description

1. Technical field [0001] The invention relates to a preparation method of a drug impurity standard product, in particular to a preparation method of an ambroxol hydrochloride impurity standard product, and belongs to the technical field of medicine. 2. Background technology [0002] Ambroxol Hydrochloride (Ambroxol Hydrochloride) is a strong expectorant, commonly used clinically for acute and chronic lung diseases accompanied by abnormal secretion of sputum and poor expectoration function, such as acute exacerbation of chronic bronchitis, Expectorant treatment of wheezing bronchitis and bronchial asthma; preventive treatment of pulmonary complications after surgery; treatment of infant respiratory distress syndrome (IRDS) in premature infants and newborns. . Ambroxol hydrochloride injection has been clinically used for many years at home and abroad. Its curative effect is definite and its quality is stable. It has been widely recognized by the market and consumers. The cli...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/74
CPCC07D239/74
Inventor 吴标张严金凌林
Owner HEFEI JIUNUO MEDICAL TECH
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