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
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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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