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A kind of method of synthesizing carbamazepine

A technology for carbamazepine and finished products, which is applied in the field of medicine and can solve problems such as the lack of synthetic carbamazepine finished products

Active Publication Date: 2018-09-04
陈建国
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this intermediate still lacks the synthetic carbamazepine finished product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Example 1, according to the weight ratio, take 20Kg of iminostilbene and 200Kg of benzene and put it into a 1000L glass-lined reaction pot for dissolution. After dissolving, react with 15Kg of triphosgene at 80°C for 6 hours to make the material react completely, and steam out 2 / 3 under reduced pressure. Benzene, after cooling, filter with suction, and dry the filter cake in a drying room at 60°C for 3-4 hours to obtain iminostilbene carboxylic acid chloride. After drying, put the filter cake into a 1000L glass-lined reaction pot and dissolve it with 300Kg of 95% ethanol. Then add 16Kg of liquid ammonia dropwise, react at 60°C for 8 hours, keep warm for 30 minutes, cool to room temperature, put in 4.5Kg of activated carbon and heat up to 78°C, decolorize for 2 hours, heat filter the mother liquor, remove the filter residue, and return the mother liquor to the glass-lined reaction In the pot, 1 / 2 of ethanol was evaporated, and after cooling, natural crystallization, sucti...

Embodiment 2

[0014] Example 2, according to the weight ratio, take 20Kg of iminostilbene and 200Kg of benzene and put it into a 1000L glass-lined reaction pot for dissolution. After dissolving, react with 14Kg of triphosgene at 80°C for 5 hours, keep the temperature for 1 hour, make the materials react completely, evaporate under reduced pressure Take out 2 / 3 benzene (measured by measuring barrel), after cooling, vacuum filter, put the filter cake in a 60°C drying room and dry for 3-4 hours to obtain iminostilbene carboxyl chloride, put the dried filter cake into 1000L enamel In a glass reaction pot, dissolve with 300Kg of 95% ethanol, then add 13Kg of liquid ammonia dropwise, react at 60°C for 8 hours, keep warm for 30 minutes, cool to room temperature, add 5Kg of activated carbon and raise the temperature to 78°C, decolorize for 2 hours, and heat filter Mother liquor, remove the filter residue, return the mother liquor to the glass-lined reaction pot, steam out 1 / 2 ethanol (measured in a ...

Embodiment 3

[0015] Example 3, according to the weight ratio, take 20Kg of iminostilbene and 200Kg of benzene and put it into a 1000L glass-lined reaction pot for dissolution. After dissolving, react with 14Kg of triphosgene at 70°C for 5 hours and keep it warm for 1 hour to make the materials react completely. 2 / 3 benzene (measured by measuring barrel), after cooling, suction filtration (vacuum filtration), the filter cake is put into a drying room at 60°C for 3-4 hours to obtain iminostilbene carboxyl chloride, which is dried Put the final filter cake into a 1000L glass-lined reaction pot (enamel glass reaction pot), dissolve it with 300Kg of 95% ethanol, then add 16Kg of liquid ammonia dropwise, react at 50°C for 8 hours, keep it warm for 30 minutes, cool to room temperature, and put in 4Kg of activated carbon Raise the temperature to 78°C, decolorize for 2 hours, heat filter the mother liquor, return the mother liquor to the glass-lined reaction pot, steam out 1 / 2 ethanol (measured in a...

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PUM

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Abstract

Provided is a method for synthesizing carbamazepine. The method comprises the steps that 1 part by weight of iminostilbene and 10 parts by weight of benzene are put into a glass lining reaction vessel of 1,000 L to be dissolved, and the materials react with 0.7 part of triphosgene for 5 h to 6 h at 70 DEG C to 80 DEG C after being dissolved to enable all the materials to react completely; 2 / 3 of benzene is distilled off through reduced pressure distillation, suction filtration is conducted after cooling is conducted, the materials are put into a drying oven or a drying room to be dried for 3 h to 4 h at 60 DEG C after being filtered, iminostilbene carbonyl chloride is obtained and put into a glass lining reaction vessel of 1,000 L, 15 parts of 95% ethyl alcohol is added, the materials are dissolved in the glass lining reaction vessel, 0.8 part of liquid ammonia is dropwise added, reacting is conducted for 8 h at 50 DEG C to 60 DEG C, heat preservation is conducted for 30 min, all the materials are cooled to room temperature, 1%-3% by weight of activated carbon is added, the temperature is increased to 78 DEG C, decoloration is conducted for 2 h, a mother solution is subjected to hot filtration, residues are discarded, and the mother solution is sent back to the glass lining reaction vessel; 1 / 2 of ethyl alcohol is distilled off, after cooling is conducted, natural crystallization and suction filtration are conducted, a crystal substance obtained after filtration is conducted is put into the drying oven or drying room to be dried for 3 h to 4 h at 60 DEG C, and the finished carbamazepine product is obtained. The yield ranges from 82% to 90%, and the content ranges from 91.5% to 99.1%.

Description

technical field [0001] The invention relates to a method for synthesizing carbamazepine, which belongs to the field of medicine. Background technique [0002] Carbamazepine is used to treat all types of epilepsy except absence seizures, to treat trigeminal neuralgia, and to prevent manic-depressive disorders. The chemical synthesis method of carbamazepine in the prior art is to obtain carbamazepine from iminodibenzyl-light (acyl chloride)-bromination-cyclization-light-light-amination. This type of synthesis method not only has many steps, The process is complex, and there is a bromination process, and bromide ions remain, so the side effects are large. The applicant once invented a method for synthesizing the iminostilbene intermediate of carbamazepine, the patent number is ZL201310205428.5, the method is as follows: the catalyst is coated on the inner wall of the reaction tube, and the outer wall of the reaction tube is covered with infrared silicon carbide The electric h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D223/22
CPCC07D223/22
Inventor 陈建国李昌平
Owner 陈建国