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Method for industrially producing mequitazine

A technology of mequitazine and phenothiazine, which is applied in the field of mequitazine preparation, can solve problems such as hydrogenation of hydrogen, achieve mild reaction conditions, be suitable for industrial production, and reduce costs and waste emissions

Active Publication Date: 2019-09-06
NINGBO SMART PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The technical problem to be solved by the present invention is to provide a method for industrialized production of mequitazine, to overcome the defect that the preparation of mequitazine from E-phenothiazine requires hydrogen hydrogenation in the prior art

Method used

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  • Method for industrially producing mequitazine

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Experimental program
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Effect test

Embodiment 1

[0034] (1) Fill the synthesis tank with nitrogen for 20-30 minutes, and at the same time, vacuum 126.8 kg of diethylene glycol dimethyl ether into a clean and dry storage tank for use. After filling with nitrogen, open the feeding port of the synthesis tank, put in 45 kg of Cl-phenothiazine and 18.5 kg of potassium tert-butoxide, and cover the feeding port. Quickly add 126.8 kg of diethylene glycol dimethyl ether from the storage tank. After adding, start stirring to make the material heat up naturally. Without heating, the material can naturally heat up to 55-65°C. When the temperature reaches 55-65°C. Keep at 55-65°C for 2 hours. After the heat preservation is completed, heat to 70° C., and after heat preservation for 1 hour, take a sample for detection (HPLC), and determine the reaction end point (MQT2≤0.2%). After the reaction is complete, add 135 kg of drinking water, heat up, and when the inner temperature reaches 90-92° C., reflux and keep warm for 30 minutes. After...

Embodiment 2

[0041] (1) Fill the 5L reaction bottle with nitrogen for 20 minutes, and at the same time, pump 1400 g of diethylene glycol dimethyl ether into a clean and dry addition funnel for use. After filling with nitrogen, put in 500g of Cl-phenothiazine and 205kg of potassium tert-butoxide, and cover the feeding port. Quickly add 1400 g of diethylene glycol dimethyl ether from the storage tank. After the addition, start the stirring, let the material exotherm and heat up naturally, and keep it at 55-65°C for 2 hours. After the heat preservation is completed, heat to 70° C., and after heat preservation for 1 hour, take a sample for detection (HPLC), and determine the reaction end point (MQT2≤0.2%). After the reaction is complete, add 1500 g of drinking water, heat up, and when the internal temperature reaches 90° C., reflux and keep warm for 30 minutes. After the heat preservation is completed, start to cool down, and when the temperature drops to 20° C., add 700 g of drinking water....

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Abstract

The invention relates to a method for industrially producing mequitazine. The method comprises the steps that under the nitrogen condition, trifluoroacetic acid and triethyl silicane are mixed, (E)-10-(1-aza bicyclic[2,2,2]cyn-3-methylene)-phenothiazine is added in batches for a reaction, water and alkali are added in sequence, extraction is performed, and an organic phase is acidified, crystallized and filtered. The method is mild in reaction condition, no high temperature or high energy dissipation is caused, solvents can be recycled, the cost is reduced, and discharge of waste is reduced.

Description

technical field [0001] The invention belongs to the field of mequitazine preparation, in particular to a method for industrial production of mequitazine. Background technique [0002] There are many synthetic methods of mequitazine reported in the literature. Among them, Cl-phenothiazine uses diethylene glycol dimethyl ether as solvent and potassium hydroxide as alkali dehalogenation (Chen Niangen, Yang Changyun, Liu Xinyong, Ren Zhaoping, Ou Shouzhen. Improvement of the synthesis process of mequitazine[J]. Chinese Medicinal Chemistry Journal, 2007 (05): 318-320.), the elimination reaction of dehalogenation can produce three isomers, and the use of inorganic bases such as potassium hydroxide will cause the formation of double bonds in the heterocycle, which will affect the target Product purity and yield. Using E-phenothiazine to generate mequitazine is the addition of double bonds by hydrogenation (Chen Niangen, Yang Changyun, Liu Xinyong, Ren Zhaoping, Ou Shouzhen. Impro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D453/02
CPCC07D453/02
Inventor 王闯顾启航殷智德向永强肖然
Owner NINGBO SMART PHARMA
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