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Crystallization process of butamidoate citrate

A technology of butamid citrate and crystallization, which is applied in the field of crystallization technology of butamid citrate, can solve the problems of long centrifugation and drying time, difficulty in removing impurities and high cost, and achieves shortening of centrifugation and drying time. Time, reduce dry loss, improve the effect of purity

Pending Publication Date: 2021-09-07
江西善渊药业有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to overcome the defects of long centrifugation and drying time, difficulty in removing impurities, low efficiency and high cost in the prior art, and provide a method that can greatly save centrifugation and drying time, have high purity, and can greatly improve efficiency and Crystallization process of butamidide citrate with low cost

Method used

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  • Crystallization process of butamidoate citrate
  • Crystallization process of butamidoate citrate
  • Crystallization process of butamidoate citrate

Examples

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Effect test

Embodiment 1

[0033] see figure 1 , a crystallization process of butamidate citrate, comprising the following process steps:

[0034] S1, mixing and dissolving: first, in the crystallization kettle, according to the quality of the alcohol solvent, the crude product of butamide citrate and the alcohol solvent are added successively according to the quality of the butamide citrate crude product 3-6 times, and the crystallization kettle The material is heated to 30-70°C, and at the same time, it is stirred until the butamidide citrate crude product is completely dissolved to obtain the first mixed solution; the alcohol solvent in step S1 is at least one of methanol, ethanol and isopropanol , preferably, the alcoholic solvent adopts isopropanol or ethanol; Preferably, the quality of the alcoholic solvent is 4-5 times of the crude product quality of butamide citrate; Preferably, the material in the crystallization tank is heated to 40 ~60°C.

[0035] S2. Crystallization: add a mixed solution o...

Embodiment 2

[0039] see figure 2 , put 30kg of crude butamidate citrate and 90kg of isopropanol into the crystallization kettle in turn, raise the temperature of the materials in the crystallization kettle to 30°C, stir until the materials are completely dissolved, then quickly drop into -15°C methanol and isopropanol The mixed solution of propyl ether is 180kg, the mass ratio of isopropanol and isopropyl ether is 1:9, the cooling rate is controlled at 10°C / h, and the stirring rate is 30r / min, so that the material in the crystallization tank is cooled to 0°C, and kept stirring for 1h , the material in the crystallization tank is subjected to solid-liquid separation through a centrifuge to obtain a filter cake and mother liquor, and the filter cake is washed with 15kg of isopropyl ether, and the washed solid is put into a dryer to dry, and the output is 29.79kg The yield of the butamide citrate crystals is 99.31%, the purity of the butamide citrate crystals reaches 99.87%, and the maximum ...

Embodiment 3

[0041] see image 3, put 30kg of crude butamidate citrate and 180kg of methanol into the crystallization tank in sequence, raise the temperature of the material in the crystallization tank to 70°C, stir until the material is completely dissolved, and quickly drop into 15°C of ethanol and methyl tert-butyl The mixed solution of ether is 300kg, the mass ratio of isopropanol and isopropyl ether is 8:2, the cooling rate is controlled at 15°C / h, and the stirring rate is 60r / min, so that the material in the crystallization tank is cooled to 5-7°C, and kept stirring 1h, the material in the crystallization tank was subjected to solid-liquid separation through a centrifuge to obtain a filter cake and mother liquor, and the filter cake was rinsed with 20kg of methyl tert-butyl ether, and the rinsed solid was put into a dryer for drying to produce Out of 29.81kg of butamidide citrate crystals, the yield is 99.37%, the purity of the butamidide citrate crystals reaches 99.87%, and the maxi...

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Abstract

The invention belongs to the technical field of chemical pharmacy, and particularly relates to a crystallization process of butamidoate citrate. The method the following steps: adding a butamil citrate crude product and an alcohol solvent into a crystallization kettle, heating, and stirring until the butamil citrate crude product is completely dissolved to obtain a first mixed solution; adding a mixed solution of an alcohol solvent and an ether solvent into the first mixed solution to obtain a second mixed solution, carrying out heat-preservation stirring, rapidly cooling the second mixed solution, and separating out crystals; performing solid-liquid separation through a centrifugal machine to obtain a filter cake; and leaching the filter cake by using a leaching solvent, and drying to obtain the butamilate citrate crystal. According to the method, the mixed solution of the alcohol solvent and the ether solvent is adopted to enable the second mixed solution to be rapidly cooled and crystallized, the obtained butamilate citrate crystals are large in granularity and loose in material, the centrifuging and drying time can be greatly shortened, the cost can be effectively reduced, impurities in a filter cake can be better removed through a leaching solvent, and the purity is effectively improved.

Description

technical field [0001] The invention belongs to the technical field of chemical industry and pharmacy, and in particular relates to a crystallization process of butamitel citrate. Background technique [0002] The situation of chronic disease prevention and control in my country is still grim. In recent years, chronic respiratory diseases have the characteristics of high prevalence, high disability rate and heavy disease burden. In the terminal market of respiratory system drugs, antitussive and expectorant cold drugs occupy a major share. Antitussive drugs include central, peripheral and facultative antitussives, butamidate citrate is a central antitussive, and its antitussive effect is 5 times stronger than that of codeine, which can promote the secretion of bronchial mucus and is suitable for the treatment of Cough caused by upper respiratory tract infection is less prone to tolerance and addiction than codeine. [0003] The structural formula of butamide citrate is as...

Claims

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Application Information

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IPC IPC(8): C07C213/10C07C217/08C07C51/42C07C59/265C07C51/43
CPCC07C213/10C07C51/42C07C51/43C07C217/08C07C59/265
Inventor 张彦军邓文正何建鹏刘超鲁红兵
Owner 江西善渊药业有限公司
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