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Chlorpheniramine maleate salifying substance and synthesis method and application thereof

The technology of a kind of chlorpheniramine acid and synthetic method is applied in the field of chlorpheniramine maleate salt formation to achieve the effects of improving purity and final yield, reducing impurity components, and reducing solvent residues

Inactive Publication Date: 2020-08-14
SHANGHAI NEW HUALIAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there is no research and development on improving the purity and yield of the intermediate chlorpheniramine maleate salify at home and abroad, therefore, it is necessary to provide new technical solutions to overcome the technical difficulties faced in the prior art

Method used

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  • Chlorpheniramine maleate salifying substance and synthesis method and application thereof
  • Chlorpheniramine maleate salifying substance and synthesis method and application thereof
  • Chlorpheniramine maleate salifying substance and synthesis method and application thereof

Examples

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Embodiment 1

[0032] Embodiment 1. A kind of preparation method of chlorpheniramine maleate salify

[0033] The present embodiment mainly describes a kind of preparation method of chlorpheniramine maleate, comprises the following steps:

[0034] Step 1. In the salt-forming kettle (1000L, glass-lined), weigh the raw material components: maleic acid 85kg, absolute ethanol 490kg, chlorpheniramine hydrolyzate 195kg and activated carbon 7kg; The raw material components are stirred, the stirring speed is 70 rpm, and the stirring time is 30 min to obtain a premix;

[0035] Step 2. Slowly heat the salt-forming kettle described in step 1 until reflux occurs at a heating rate of 2.5°C / min, and keep refluxing for 1 hour when heated to 80°C to obtain a heated feed liquid;

[0036] Step 3. Under heat preservation conditions, transfer the heated feed liquid obtained in Step 2 from the salt-forming kettle to a filter press (300L, stainless steel), and then press it from the filter press to the crystalliz...

Embodiment 2

[0044] Embodiment 2. A kind of preparation method of chlorpheniramine maleate salify

[0045] The present embodiment mainly describes a kind of preparation method of chlorpheniramine maleate salt, comprising the following steps:

[0046] Step 1. Add 190kg of chlorpheniramine hydrolyzate, 460kg of absolute ethanol, and then add 80kg of maleic acid and 4kg of activated carbon in a salt-forming kettle (1000L, glass-lined), and stir at a speed of 65 rpm , and the stirring time was 40 min to obtain a premix;

[0047] Step 2. Slowly heat the salt-forming kettle described in step 1 until reflux occurs at a heating rate of 1°C / min, and keep reflux at 75°C for 1.5 hours to obtain a heating feed liquid;

[0048] Step 3. Under the condition of heat preservation, transfer the heated feed liquid obtained in step 2 from the salt forming kettle to the filter press kettle (300L, stainless steel), and then use nitrogen to press from the filter press kettle to the crystallization kettle, and k...

Embodiment 3

[0055] Embodiment 3. A kind of preparation method of chlorpheniramine maleate salt

[0056] The present embodiment mainly describes a kind of preparation method of chlorpheniramine maleate salt, comprising the following steps:

[0057] Step 1. Add 210kg of chlorpheniramine hydrolyzate and 530kg of absolute ethanol to the salt-forming kettle (1000L, glass-lined), then add 90kg of maleic acid and 10kg of activated carbon for stirring at a stirring speed of 90 rpm , and the stirring time was 20 min to obtain a premix;

[0058] Step 2. Slowly heat the salt-forming kettle described in step 1 until reflux occurs, the heating rate is 5°C / min, and keep reflux at 85°C for 0.8 hours to obtain the heating feed liquid;

[0059] Step 3. Under heat preservation conditions, transfer the heated feed liquid obtained in Step 2 from the salt-forming kettle to a filter press (300L, stainless steel), and then press from the filter press to the crystallization kettle), and keep the nitrogen pressu...

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Abstract

The invention provides a chlorpheniramine maleate salifying substance and a synthesis method and application thereof. The synthesis method comprises the following steps: weighing the following raw material components in parts by weight: 80-90 parts of maleic acid, 460-530 parts of absolute ethyl alcohol, 190-210 parts of chlorpheniramine hydrolysate, 4-10 parts of activated carbon and the like, then stirring and mixing the weighed raw material components to obtain a preheated mixture, transferring the preheated mixture into a filter pressing kettle, carrying out filter pressing and purification to obtain a filter pressing feed liquid of a crystallization kettle, cooling the filter pressing feed liquid of the crystallization kettle, carrying out centrifugal filtration, flushing by absoluteethyl alcohol after filtration, carrying out centrifugation again to obtain the chlorpheniramine maleate salifying substance. By adopting the synthesis method disclosed by the invention, the purity and the final yield of the synthesized chlorpheniramine maleate salifying substance are improved, and the impurity content of the chlorpheniramine maleate salifying substance is reduced.

Description

technical field [0001] The invention belongs to the field of pharmacy, and in particular relates to a chlorpheniramine maleate salt, its synthesis method and application. Background technique [0002] Chlorpheniramine maleate is an antihistamine drug, which plays an anti-allergic effect by antagonizing H1 receptors. It is mainly used for rhinitis, skin and mucous membrane allergies, and relief of cold symptoms such as tearing, sneezing, and runny nose. , the market demand is large. Yet, in the preparation process of chlorpheniramine maleate, the purity and the yield of its precursor chlorpheniramine maleate salify play a vital role to the preparation of later stage chlorpheniramine maleate . [0003] At present, there is no research and development on improving the purity and yield of the intermediate chlorpheniramine maleate salify at home and abroad, therefore, it is necessary to provide new technical solutions to overcome the technical difficulties faced in the prior ar...

Claims

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Application Information

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IPC IPC(8): C07D213/38C07C51/43C07C51/42C07C51/41C07C57/145
CPCC07D213/38C07C51/412C07C51/42C07C51/43C07C57/145
Inventor 卿文彬柏挺周秋火华吉涛金芳
Owner SHANGHAI NEW HUALIAN PHARMA
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