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Method for preparing meclofenoxate hydrochloride

A technology of meclofenoxate hydrochloride and ethyl acetate, applied in the field of preparation of central nervous system stimulant meclofenoxate hydrochloride, can solve the problems of harsh reaction conditions, cumbersome operation steps, unsuitable for industrialization, etc., and achieve good powder shape , Improve the reaction yield, the effect of large production capacity

Active Publication Date: 2019-07-16
GUANGDONG XIANQIANG PHARMA +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The method uses toluenesulfonic acid, a highly corrosive strong acid, and requires azeotropic water separation under toluene conditions, and then requires low-temperature crystallization, which is not easy to operate. When thionyl chloride is excessive, the pollution is relatively large, and subsequent hydrochloride formation is not possible. Sufficient problem, and the yield is only 70%, not suitable for industrialization
[0014] In summary, the preparation of meclofenoxate hydrochloride in the prior art mostly uses highly toxic and highly corrosive reagents, the reaction conditions are relatively harsh, the operation steps are cumbersome, and the product purity and yield are not ideal.

Method used

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  • Method for preparing meclofenoxate hydrochloride
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  • Method for preparing meclofenoxate hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (A) Put p-chlorophenoxyacetic acid (50g, 0.26mol) into 500ml ethyl acetate in a single-necked bottle, then add dimethylaminoethanol (25.4g, 0.29mol), stir at room temperature for 20min, and finally add the condensing agent EDCI ( 55.4g, 0.29mol), stirred and reacted at 25°C for 3h;

[0038] (B) Add 200ml of water after the reaction to quench, extract and separate layers, and the organic layer is converted into hydrochloride by hydrogen chloride gas. The flow rate of hydrogen chloride gas is 15m / s, until a large amount of solids are precipitated, and slowly stirred at 25°C for 2h to crystallize. Filter and dry to obtain 67g of white solid, with a yield of 87.6%, a purity of 99.7%, and a bulk density of 0.51g / cm 3 , the angle of repose is 28°, the powder is loose and the viscosity is weak.

Embodiment 2

[0040] (A) Put p-chlorophenoxyacetic acid (50g, 0.26mol) into 250ml of dichloromethane in a single-necked bottle, then add dimethylaminoethanol (20.1g, 0.23mol), stir at room temperature for 10min, and finally add the condensing agent DCC ( 47.3g, 0.23mol), stirred and reacted at 25°C for 1h;

[0041] (B) Add 100ml of water after the reaction to quench, extract and separate layers, and the organic layer is formed into hydrochloride by hydrogen chloride gas. The flow rate of hydrogen chloride gas is 10m / s, until a large amount of solids are precipitated, and slowly stirred at 10°C for 1h to crystallize. Filter and dry to obtain 64g of white solid, the yield is 83.7%, the purity is 99.7%, and the bulk density is 0.55g / cm 3 , the angle of repose is 30°, the powder is loose and the viscosity is weak.

Embodiment 3

[0043] (A) Put p-chlorophenoxyacetic acid (50g, 0.26mol) into 1000ml ethyl acetate in a single-necked bottle, then add dimethylaminoethanol (27.2g, 0.31mol), stir at room temperature for 30min, and finally add the condensing agent CDI ( 55.0g, 0.34mol), stirred and reacted at 25°C for 5h;

[0044] (B) Add 250ml of water after the reaction to quench, extract and separate the layers, and the organic layer is converted into hydrochloride by hydrogen chloride gas. The flow rate of hydrogen chloride gas is 18m / s, until a large amount of solids are precipitated, and slowly stirred at 30°C for 3h to crystallize. Filter and dry to obtain 66g of white solid, the yield is 86.3%, the purity is 99.8%, and the bulk density is 0.58 / cm 3 , the angle of repose is 32°, the powder is loose and the viscosity is weak.

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Abstract

The invention discloses a method for preparing meclofenoxate hydrochloride. A reaction route is as follows: carrying out a reaction under moderate conditions by using CDI or EDCI or DCC or the like asa condensing agent. According to the method, the operation is simple, convenient, safe and environmentally friendly, meanwhile, a decolorization process in the prior art is avoided, and then, the yield of reaction is increased; and the finished product has no need of recrystallization and is high in purity, stable in quality and good in powder form, so that a process of drying a solvent by distillation in the prior art is avoided, the operation is simple, solvent recovery is facilitated, industrialization is easy to achieve, and the production capacity is large.

Description

technical field [0001] The invention belongs to the field of chemical synthesis. Specifically, the invention relates to a preparation method of meclofenoxate hydrochloride, a central nervous stimulant. Background technique [0002] Meclofenoxate hydrochloride (Meclofenoxate hydrochloride), CAS: 3685-84-5, the trade name is chlorate aldehyde, and the chemical name is dimethylaminoethyl p-chlorophenoxyacetate hydrochloride (2-(dimethylamino)ethyl 4- chlorophenoxyacetate hydrochoride), the chemical structural formula is as follows: [0003] [0004] Meclofenoxate hydrochloride mainly acts on the cerebral cortex. It can promote the redox of brain cells, regulate the metabolism of nerve cells, increase the utilization of carbohydrates and have an excitatory effect on the inhibited central nervous system. Treatment of traumatic coma, enuresis in children, disturbance of consciousness, senile mental illness, various dementias, alcoholism, etc. [0005] At present, the domestic...

Claims

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Application Information

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IPC IPC(8): C07C219/06C07C213/06C07C213/08
CPCC07C213/06C07C213/08C07C219/06
Inventor 熊伟梅邓军黎万黄彩逢罗日康谭珍友
Owner GUANGDONG XIANQIANG PHARMA