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Preparation method of mebhydrolin napadisylate

A technology of heltraline naphthalene disulfonic acid and sodium naphthalene disulfonate, which is applied in the field of preparation of mehaitraline naphthalene disulfonic acid, and can solve the problems of product quality failing to meet requirements, high sulfate ion concentration, and incomplete conversion reaction and other problems, to achieve the effect of stable improvement of product quality, improvement of reaction yield, and improvement of total reaction yield

Inactive Publication Date: 2019-05-31
辽宁博美医药科技有限公司
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  • Claims
  • Application Information

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Problems solved by technology

[0006] The actual operation found that in the last step of the method, the conversion reaction from sulfate to sulfonic acid was not complete, the concentration of sulfate ions in the final product was high, the product was difficult to refine, and the product quality could not meet the requirements

Method used

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  • Preparation method of mebhydrolin napadisylate
  • Preparation method of mebhydrolin napadisylate
  • Preparation method of mebhydrolin napadisylate

Examples

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Effect test

Embodiment 1

[0024] (1) Preparation of N-methyl-4-piperidone hydrochloride solution

[0025] Add 250ml of xylene and 20.0g of methylimine-N,N-dipropionate into the reaction kettle, then add 9.5g of solid sodium methoxide after cooling down, stir and heat under reflux for 4 hours until the reaction is complete. Lower the temperature of the reactants in the previous step to 40°C, add 10ml of water, stir to completely dissolve, add 30ml of concentrated hydrochloric acid, stir for 10 minutes, and let stand to separate layers (the bottom layer will have a small amount of white insoluble matter, which is a normal phenomenon). Separate the xylene layer, extract the xylene once with 30ml of concentrated hydrochloric acid, combine the hydrochloric acid layers, and heat the hydrochloric acid layer to reflux for decarboxylation for 5 hours to obtain N-methyl-4-piperidone hydrochloride solution, containing about 10.0g of product. The yield was 90%, and the solution went directly to the next step witho...

Embodiment 2

[0031] (1) Preparation of N-methyl-4-piperidone hydrochloride solution

[0032] Add 250ml of toluene and 20g of methylimine-N,N-dipropionate into the reaction kettle, then cool down and add 48.9g of 28% liquid sodium methoxide, stir and heat under reflux for 10 hours until the reaction is complete. Lower the temperature of the reactants in the previous step to 40°C, add 10ml of water, stir to completely dissolve, add 30ml of concentrated hydrochloric acid, stir for 10 minutes, and let stand to separate layers (the bottom layer will have a small amount of white insoluble matter, which is a normal phenomenon). Separate the toluene layer, extract the toluene once with 30ml of concentrated hydrochloric acid, combine the hydrochloric acid layers, and heat the hydrochloric acid layer to reflux for decarboxylation for 5 hours to obtain N-methyl-4-piperidone hydrochloride solution, containing about 9.0g of the product. The calculated yield is 81 %, the solution went directly to the ne...

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Abstract

The invention belongs to the field of drug synthesis and provides a preparation method of mebhydrolin napadisylate. The preparation method is characterized by including the steps of firstly, subjecting methyl imine-N,N-methyl dipropionate and sodium methylate to heating under the effect of an organic solvent to achieve loop closing, and using hydrochloric acid to performing heating decarboxylationto obtain N-methyl-4-piperidone hydrochloride; subjecting phenylhydrazine and benzyl chloride to condensation under an alkaline condition to obtain benzyl phenylhydrazine; thirdly, mixing the N-methyl-4-piperidone hydrochloride solution and the benzyl phenylhydrazine, heating to generate mebhydrolin hydrochloride, adding disodium 1,5-naphthalenedisulfonate to obtain the mebhydrolin napadisylate.The preparation method is high in yield, mild in reaction conditions, convenient in intermediate purification and capable of satisfying the requirements of industrial production.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of mehaltraline naphthalene disulfonic acid. Background technique [0002] Mehetraline naphthalene disulfonic acid is a new generation of antihistamines, clinically used for hives, rhinitis, angioedema and serum sickness, the anti-allergic effect is 10 times that of chlorpheniramine. But in our country, such drugs are basically dependent on imports. With the continuous expansion of the pilot scope of the basic medical insurance system for urban residents, the comprehensive promotion of new rural cooperative medical care, and the introduction and implementation of a new round of medical and health system reform plans, the huge potential of the domestic pharmaceutical consumption market has gradually become prominent, which has effectively promoted the overall level of medical care. upgrade. The advancement of medicine and the increase in the prop...

Claims

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Application Information

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IPC IPC(8): C07D471/04
Inventor 周小明姜雨李伟刘勇王倩
Owner 辽宁博美医药科技有限公司
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