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Eperisone hydrochloride production method

A technology of eperisone hydrochloride and its production method, which is applied in the field of production of eperisone hydrochloride, can solve problems such as no patent registration for eperisone hydrochloride, and achieve the effects of preventing waste, simple operation, and comprehensive process

Active Publication Date: 2013-08-07
HUNAN YADA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Through the patent search, there is no patent report for the production method of Eperisone Hydrochloride

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0017] A kind of production method of eperisone hydrochloride is characterized in that comprising following processing steps:

[0018] Step a, preparation of piperidine hydrochloride: take 2.1 kg of piperidine, put it into 2.8 kg of absolute ethanol, start stirring, add 3.4 kg of concentrated hydrochloric acid with a mass fraction of 37% or more dropwise, and control the temperature during the reaction Below 90°C, pH 2 is the end point of the reaction; after the reaction, ethanol is recovered, cooled to 8°C for crystallization, and centrifuged to obtain piperidine hydrochloride;

[0019] Step b. Synthesis of Mannich base: Take 1.6kg of isopropanol, 3.6kg of p-ethylpropiophenone, 2.6kg of piperidine hydrochloride, and 0.7kg of paraformaldehyde, put them in order and stir evenly, at 95°C Reflux for 5 hours, recover isopropanol after the reaction is complete, then add 10 kg of water while it is hot, stir, dissolve, cool, extract with 2 kg of isopropyl ether, remove impurities twi...

Embodiment 2

[0024] A kind of production method of eperisone hydrochloride is characterized in that comprising following processing steps:

[0025] Step a, preparation of piperidine hydrochloride: take 2.1 kg of piperidine, put it into 2.8 kg of absolute ethanol, start stirring, add dropwise 3.4 kg of concentrated hydrochloric acid with a mass fraction of 37% or more, and control the temperature during the reaction Below 90°C, pH 5 is the end point of the reaction; after the reaction, ethanol is recovered, cooled to 10°C for crystallization, and centrifuged to obtain piperidine hydrochloride;

[0026] Step b, Synthesis of Mannich base: Take 1.6kg of isopropanol, 3.6kg of p-ethylpropiophenone, 2.6kg of piperidine hydrochloride, and 0.7kg of paraformaldehyde, put them in order and stir evenly, at 100°C Reflux for 5 hours, recover isopropanol after the reaction is complete, then add 10kg of water while it is hot, stir, dissolve, cool, extract with 2kg of isopropyl ether, remove impurities twi...

Embodiment 3

[0031] A kind of production method of eperisone hydrochloride is characterized in that comprising following processing steps:

[0032] Step a, preparation of piperidine hydrochloride: take 2.1 kg of piperidine, put it into 2.8 kg of absolute ethanol, start stirring, add dropwise 3.4 kg of concentrated hydrochloric acid with a mass fraction of 37% or more, and control the temperature during the reaction Below 90°C, pH3 is the end point of the reaction; after the reaction, ethanol is recovered, cooled to 9°C for crystallization, and centrifuged to obtain piperidine hydrochloride;

[0033] Step b, Synthesis of Mannich base: Take 1.6kg of isopropanol, 3.6kg of p-ethylpropiophenone, 2.6kg of piperidine hydrochloride, and 0.7kg of paraformaldehyde, put them in order and stir evenly, at 98°C Reflux for 5 hours, recover isopropanol after the reaction is complete, then add 10kg of water while it is hot, stir, dissolve, cool, extract with 2kg of isopropyl ether, remove impurities twice,...

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PUM

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Abstract

The invention discloses an eperisone hydrochloride production method. The method comprises four technological steps, wherein effectively preparing piperidine hydrochloride is prepared through step a; mannich base is further synthesized through step b; a crude eperisone hydrochloride product is obtained by step c; and the eperisone hydrochloride is finely produced by step d. The method can be adopted to produce effective ingredients to the maximum extent, the total recovery reaches above 75%, and the effective ingredients can be prevented from being wasted. Moreover, the method is technologically comprehensive and convenient to operate, and the eperisone hydrochloride can be conveniently and industrially produced.

Description

technical field [0001] The present invention relates to the production technology method of medicine, particularly a kind of production method of eperisone hydrochloride. Background technique [0002] Eperisone hydrochloride is a central muscle relaxant, which is used to improve the muscle tension of neck, shoulder and arm syndrome, periarthritis of shoulder, and low back pain, and at the same time improve cerebrovascular disorders, cervical spondylosis, sequelae of surgery, sequelae of trauma, muscle tension, etc. Atrophic lateral sclerosis, infantile cerebral palsy, spinocerebellar degeneration, spinal vascular disorders, spastic paralysis of subacute spinal neuropathy. [0003] The invention involves three key steps, one is the preparation of piperidine hydrochloride, the other is the synthesis of Mannich base, and the third is the salt formation of eperisone. Through patent retrieval, the production method of eperisone hydrochloride still has no patent report at present...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/104
Inventor 张海武
Owner HUNAN YADA PHARMA
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