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Production method of mexiletine hydrochloride

A technology of mexiletine hydrochloride and a production method, applied in the production field of mexiletine hydrochloride, can solve the problems of removal of difficult mixtures, difficulty in recovery and purification, and high price, and achieves the effects of increasing production rate, reducing production cost, and less resource consumption

Inactive Publication Date: 2018-01-30
CHANGZHOU YABANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] All there are more deficiencies in the above-mentioned two kinds of production techniques, in the first kind of production technique, have used highly poisonous sodium dichromate and have therefore introduced polluting discharge; In the second kind of production technique, used when preparing ether ketone Solid-liquid two-phase reaction, using a high-boiling polar aprotic solvent dimethylformamide (DMF) as a reaction solvent to dissolve salts and organics, but the polar aprotic solvent used generally has a higher boiling point, and at the end of the reaction It is difficult to remove from the mixture afterward, and recovery and purification are difficult, and the price is much higher than that of ordinary alcohols and hydrocarbons

Method used

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  • Production method of mexiletine hydrochloride
  • Production method of mexiletine hydrochloride
  • Production method of mexiletine hydrochloride

Examples

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Effect test

Embodiment 1

[0043] Etherification step: put 122 parts of 2,6-dimethylphenol and 366 parts of 1,2-dichloroethane into the reactor, add 61 parts of potassium carbonate, 3 parts of sodium bromide, 16 parts of tetrabutyl bromide ammonium chloride, the temperature was raised to reflux, and a mixed solution of 40 parts of 1,2-dichloroethane and 80 parts of chloroacetone was added dropwise, and the reflux reaction was continued for 2 hours after dropping. The solid residue was filtered off, and 1,2-dichloroethane was recovered to obtain 170 parts of ether ketone.

[0044] Amination reduction step: put 170 parts of sperm ketone, 385 parts of 10% ammonia methanol, and 6 parts of Raney nickel into the hydrogenation kettle, feed hydrogen into the kettle to 1.2MPa, raise the temperature to 100°C, keep warm and keep the hydrogen pressure at 1.2 MPa, until the end of hydrogen absorption, the temperature is lowered to below 30°C, the catalyst is removed by sedimentation, and the ammonia methanol is reco...

Embodiment 2

[0047] Etherification step: Put 120 parts of 2,6-dimethylphenol and 360 parts of 1,2-dichloroethane into the reaction kettle, add 200 parts of potassium bicarbonate, 2 parts of potassium iodide, and 10 parts of tetrabutylammonium bromide , the temperature was raised to reflux, and a mixed solution of 600 parts of 1,2-dichloroethane and 70 parts of chloroacetone was added dropwise, and the reflux reaction was continued for 2 hours after dropping. The solid residue was filtered off, and 1,2-dichloroethane was recovered to obtain 170 parts of ether ketone.

[0048] Amination reduction step: put 170 parts of sperm ketone, 342 parts of 10% ammonia methanol, and 11.4 parts of Raney nickel into the hydrogenation kettle, feed hydrogen into the kettle to 1.2MPa, raise the temperature to 100°C, keep warm and keep the hydrogen pressure at 1.2 MPa, until the end of hydrogen absorption, the temperature is lowered to below 30°C, the catalyst is removed by sedimentation, and the ammonia meth...

Embodiment 3

[0051] Etherification step: Put 130 parts of 2,6-dimethylphenol and 370 parts of 1,2-dichloroethane into the reactor, add 80 parts of potassium carbonate, 5 parts of sodium bromide, 20 parts of tetrabutyl bromide ammonium, the temperature was raised to reflux, and a mixed solution of 40 parts of 1,2-dichloroethane and 90 parts of chloroacetone was added dropwise, and the reflux reaction was continued for 2 hours after dropping. The solid residue was filtered off, and 1,2-dichloroethane was recovered to obtain 175 parts of ether ketone.

[0052] Amination reduction step: Put 175 parts of sperm ketone, 405 parts of 10% ammonia methanol, and 7 parts of Raney nickel into the hydrogenation kettle, feed hydrogen into the kettle to 1.2MPa, raise the temperature to 100°C, keep warm and keep the hydrogen pressure at 1.2 MPa, until the hydrogen absorption is completed, the temperature is lowered to below 30°C, the catalyst is removed by sedimentation, and the ammonia methanol is recover...

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Abstract

The invention provides a production method of mexiletine hydrochloride. The method comprises: a etherification step, namely dissolving 2,6-dimethylphenol in a solid-liquid heterogeneous reaction system to obtain a mixed solution, mixing chloroacetone with the mixed solution, and performing reflux reaction to obtain ether ketone, wherein the solid-liquid heterogeneous reaction system comprises a solvent, a solid-liquid phase transfer promoter, inorganic base and an alkali metal halide; an amination reduction step, namely under suitable reaction conditions, contacting the ether ketone with ammonia methanol to carry out amination reduction reaction to obtain ether amine; and a salting step, namely reacting the ether amine with hydrogen chloride in the solvent to obtain the mexiletine hydrochloride. The method disclosed by the invention improves the reaction efficiency and the production efficiency, and has the advantages of low production cost, small resource consumption and high production efficiency.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and generally relates to a production method of mexiletine hydrochloride. Background technique [0002] Mexiletine Hydrochloride, English name: Mexiletine Hydrochloride, commonly known as slow heart rhythm, chemical name: (±)-1-(2,6-dimethylphenoxy)-2-propanamine hydrochloride (CAS No: 5370-01 -4), molecular formula: C 11 h 17 NO·HCl, molecular weight: 215.72, structural formula as follows: [0003] [0004] The structure of mexiletine hydrochloride is similar to that of lidocaine. It was initially found to have anticonvulsant effect. Later, it was proved that the drug has a good effect on arrhythmia caused by coronary artery ligation. Currently, it is mainly used clinically to treat acute and chronic ventricular arrhythmia Arrhythmia. [0005] At present, there are mainly two kinds of processes in China to produce mexiletine hydrochloride. The first one is to obtain ether alcoh...

Claims

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Application Information

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IPC IPC(8): C07C45/64C07C49/255C07C213/02C07C213/08C07C217/18
Inventor 陶锋徐树行夏正君王剑李伟亮
Owner CHANGZHOU YABANG PHARMA
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