A kind of method for industrialized production of 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, reduce equipment requirements and safety risks, and be suitable for industrial production

Active Publication Date: 2022-06-24
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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  • A kind of method for industrialized production of mequitazine

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Embodiment 1

[0034] (1) First fill the synthesis tank with nitrogen for 20-30 minutes, and at the same time, vacuum 126.8kg 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 126.8kg of diethylene glycol dimethyl ether from the storage tank. After adding, start stirring to make the material naturally exothermic and heat up. Without heating, the natural exothermic temperature of the material can reach 55-65°C. When the temperature reaches 55-65℃. Keep at 55-65°C for 2 hours. After the incubation, the mixture was heated to 70° C., and after 1 hour of incubation, sampling was performed for detection (HPLC) to determine the reaction end point (MQT2≤0.2%). After the reaction was completed, 135 kg of drinking water was added, and the temperature was heated up. When the internal tem...

Embodiment 2

[0041] (1) Fill the 5L reaction flask 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 later use. After filling with nitrogen, put in 500 g of Cl-phenothiazine and 205 kg 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, the stirring was started, and the material was naturally exothermic and heated, and the temperature was kept at 55-65 °C for 2 hours. After the incubation, the mixture was heated to 70° C., and after 1 hour of incubation, sampling was performed for detection (HPLC) to determine the reaction end point (MQT2≤0.2%). After the reaction was completed, 1500 g of drinking water was added, and the temperature was heated up. When the internal temperature reached 90° C., the mixture was refluxed for 30 minutes. After the heat preservation is completed, start to cool down. Whe...

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Abstract

The invention relates to a method for industrialized production of mequitazine. The method comprises: under nitrogen condition, trifluoroacetic acid and triethylsilane are mixed, and (E)‑10‑(1‑azabicyclo[2,2,2]octyl‑3‑ylidenemethyl)‑ For phenothiazine reaction, add water and alkali in sequence, extract, acidify the organic phase, crystallize, and filter. The method has mild reaction conditions, no high temperature and high energy consumption, the solvent can be recovered, and the cost and waste discharge are reduced.

Description

technical field [0001] The invention belongs to the field of mequitazine preparation, in particular to a method for industrialized production of mequitazine. Background technique [0002] There are many synthetic methods of mequitazine reported in the literature. Among them, Cl-phenothiazine is dehalogenated with diethylene glycol dimethyl ether as solvent and potassium hydroxide as alkali (Chen Niangen, Yang Changyun, Liu Xinyong, Ren Zhaoping, Ou Shouzhen. Improvement of the synthesis process of mequitazine [J]. China Medicinal Chemistry Journal, 2007(05): 318-320.), dehalogenation and elimination reaction 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. The use of E-phenothiazine to generate mequitazine is the addition of hydrogen hydrogenation to the double bond (Chen Niangen, Yang Changyun, Liu Xinyong, Ren Zhaoping, ...

Claims

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Application Information

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Patent Type & Authority Patents(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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