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Method for preparing hydrochloride urapidil

A technology of uradil hydrochloride and uradil, applied in the direction of organic chemistry, can solve the problems of unqualified product content, pH, clarity, difficult pH control, etc., and achieve the effect of simple method, easy operation and stable quality

Inactive Publication Date: 2008-06-18
YAOPHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Because in the prior art, the preparation of urapidil hydrochloride is obtained by dissolving uradil in a solvent system and feeding hydrochloric acid gas into salt and crystallization, in this preparation process, the pH of the product is difficult to control, and a little improper operation may cause Cause the content, pH, clarity and other indicators of the product to be unqualified

Method used

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  • Method for preparing hydrochloride urapidil
  • Method for preparing hydrochloride urapidil
  • Method for preparing hydrochloride urapidil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In a 250mL three-necked flask equipped with a reflux condenser, add 160ml of absolute ethanol and 8.1g of urapidil refined product, heat to 90°C while stirring, and dropwise add hydrogen chloride ethanol solution (obtained by passing hydrogen chloride gas into ethanol solvent) Use precision pH test paper to control the pH of the solution at about 3-4, continue to stir and keep warm for 30 minutes, the system is still a clear and transparent solution, then slowly cool down to about 40°C, crystallize at constant temperature for 1 hour, heat filter, and use the filter cake Wash once with a small amount of absolute ethanol, and filter with suction. The filter cake was dried under reduced pressure and <60°C for 2 hours to obtain 6.6 g of white crystalline urapidil hydrochloride, with a yield of 75.4%, a total yield of 61.1% (theoretical value 10.9 g), and a content of 100.5 g in dry terms. %, related substances are 0.02%, pH=4.76, clarity <No. 2 standard turbidity liquid.

Embodiment 2

[0022] In a 250mL three-necked flask equipped with a reflux condenser, add 160ml of absolute ethanol and 8.1g of urapidil refined product, heat to 80°C under stirring, and dropwise add hydrogen chloride ethanol solution (obtained by passing hydrogen chloride gas into ethanol solvent) Use precision pH test paper to control the pH of the solution at 2-3, continue to stir and keep warm for 30 minutes, the system is still a clear and transparent solution, then slowly cool down to about 70°C, add an appropriate amount of urapidil hydrochloride seed crystals, and crystallize at constant temperature After 1 hour, hot filter, the filter cake was washed once with a small amount of absolute ethanol, and suction filtered. The filter cake was dried under reduced pressure at <60°C for 2 hours to obtain 4.1 g of white crystalline urapidil hydrochloride, with a yield of 37.6%, a dry product content of 101.0%, related substances 0.05%, pH=4.39, Clarity <No. 2 standard turbidity liquid.

Embodiment 3

[0024] In a 250mL three-necked flask equipped with a reflux condenser, add 160ml of absolute ethanol and 8.1g of urapidil refined product, heat to 60°C under stirring, and dropwise add hydrogen chloride ethanol solution (obtained by passing hydrogen chloride gas into ethanol solvent) Use precision pH test paper to control the pH of the solution at about 3-4, continue to stir and keep warm for 30 minutes, the system is still a clear and transparent solution, then slowly cool down to about 40°C, add a small amount of urapidil hydrochloride seed crystals, and analyze at constant temperature Crystallize for 1 hour, heat filter, wash the filter cake once with a small amount of absolute ethanol, and filter with suction. The filter cake was dried under reduced pressure at <60°C for 2 hours to obtain 7.7 g of white crystalline urapidil hydrochloride, with a yield of 70.6%, a dry product content of 99.9%, related substances of 0.02%, pH=5.12, Clarity <No. 2 standard turbidity liquid. ...

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Abstract

The invention relates to a preparation method of the urapidil hydrochloride. The method comprises the following procedures, the urapidil is dissolved in the alcohols or / and the ketones solvent, the organic solution of the hydrogen chloride is slowly added after the heating dissolution for controlling pH at the range of 2.0 to 4.0, then the mixture is crystallized by decreasing the temperature into the range of 20 to 70 DEG C, and the urapidil hydrochloride is filtrated and dried by the decompression drying. The content is not lower than 99.5 percent, the clarity and the pH meet the purity requirement of the raw material used in the injection. The invention has the advantages of simple method, stable quality, easy operation and being suitable for the industrial production.

Description

technical field [0001] The invention relates to a preparation method of urapidil hydrochloride. Background technique [0002] The chemical name of urapidil hydrochloride is 6-[[3-[4-(2-methoxyphenyl)-1-piperazinyl]propyl]amino]-1,3-dimethyl-2,4 (1H, 3H) pyridildione hydrochloride, the English name is Urapidil Hydrochloride, and the English chemical name is 6-[[3-[4-(2-Methoxyphenyl)-1-piperazinyl]propyl]amino]-1,3 -Dimethy1-2,4(1H,3H)-pyrimi dinedione Hydrochloride, its chemical structural formula: [0003] [0004] The trade names of urapidil hydrochloride are Urapil, Ebrantil, and Lixidine, which are uracils substituted by oxazosin. This product has both peripheral and central hypotensive effects. Peripheral mainly blocks the post-synaptic α1 receptors, causing vasodilation to significantly reduce peripheral resistance. At the same time, it also has a weak presynaptic α2 blocking effect, blocking the vasoconstrictive effect of catecholamines (different from the perip...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/545
Inventor 刘永红李静谭俊杰
Owner YAOPHARMA CO LTD
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