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Preparation method of high-purity vortioxetine hydrobromide

A technology of vortioxetine hydrobromide and vortioxetine, which is applied in the field of preparation of high-purity vortioxetine hydrobromide, can solve the problem of high purity of vortioxetine hydrobromide and the production purity of vortioxetine Low cost, high cost, etc., to achieve the effects of easy industrial production, high product yield, and mild process reaction conditions

Active Publication Date: 2015-06-24
郑州大明药物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the invention is to provide a kind of preparation method of high-purity vortioxetine hydrobromide for the problems such as low purity and high cost of vortioxetine in the prior art. The method adopts low raw material price, low cost, The process is simple, and the produced vortioxetine hydrobromide has high purity and less impurities

Method used

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  • Preparation method of high-purity vortioxetine hydrobromide

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Embodiment 1

[0024] Embodiment 1: This embodiment provides a kind of preparation method of high-purity vortioxetine hydrobromide, and concrete steps are as follows:

[0025] Step 1: Synthesis of 2-(2,4-dimethylphenylsulfanyl) chlorobenzene:

[0026]

[0027] Get a 250ml reaction bottle, feed nitrogen into the bottle, get 20g (0.16mol) of 2-chlorophenol (formula I) and 21.5g (0.16mol) of 2,4-dimethylthiophenol (formula II) and add to the reaction Add 135.3g of ethyl acetate, 0.9g (0.016mol) of nickel nanopowder, 39.4g (0.48mol) of sodium isopropoxide and 10g of anhydrous sodium sulfate into the bottle, stir at room temperature for 20min, raise the temperature to 50°C, and stir for 8h , TLC to monitor the reaction process, after the reaction is over, stop heating, and filter the reaction solution after it drops to room temperature, wash the filtrate 3 times, 50ml each time, take the organic phase, add anhydrous sodium sulfate to dry overnight, filter, and the filtrate is rotated The solv...

Embodiment 2

[0035] Embodiment 2: This embodiment provides another kind of preparation method of high-purity vortioxetine hydrobromide, and concrete steps are as follows:

[0036] Step 1: Synthesis of 2-(2,4-dimethylphenylsulfanyl) chlorobenzene:

[0037]

[0038] Get a 500ml reaction bottle, feed nitrogen into the bottle, get 30g (0.24mol) of 2-chlorophenol (formula I) and 32.25g (0.24mol) of 2,4-dimethylthiophenol (formula II) into the reaction Add 202.95g of ethyl acetate, 1.35g (0.024mol) of nickel nanopowder, 59.1g (0.72mol) of sodium isopropoxide and 15g of anhydrous sodium sulfate into the bottle, stir at room temperature for 23min, raise the temperature to 55°C, and stir for 9h , TLC to monitor the reaction process, after the reaction is over, stop heating, and filter the reaction solution after it drops to room temperature (20-25°C), wash the filtrate with water 3 times, 60ml each time, take the organic phase, add anhydrous sodium sulfate to dry overnight , filtered, and the f...

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Abstract

The invention discloses a preparation method of high-purity vortioxetine hydrobromide. The method comprises the following steps: firstly, synthesizing 2-(2,4-dimethyl phenyl sulfanyl) chlorobenzene from 2-chlorophenol and 2,4-dimethylbenzenethiol; then, adding di(dibenzylideneacetone)palladium, 1,1'-binaphthyl-2,2'-bis(diphenyl phosphine), sodium tert-butoxide, and methylbenzene into a reaction bottle to mix, and adding other materials so as to prepare vortioxetine; and dissolving the prepared vortioxetine by using 14-16 times of ethyl acetate, so that a vortioxetine hydrobromide coarse product is obtained; and finally, purifying the coarse product so as to obtain a vortioxetine hydrobromide fine-product. The method disclosed by the invention is easily-obtained in raw materials, mild in process reaction conditions, high in product yield, high in product purity, and convenient for industrial production. Prepared vortioxetine hydrobromide is white crystalline powder, and the purity is more than 99.5%.

Description

technical field [0001] The invention relates to the field of drug synthesis, in particular to a preparation method of high-purity vortioxetine hydrobromide. Background technique [0002] Vortioxetine is a new type of antidepressant drug developed by Lundbeck Pharmaceutical Company of Denmark and Takeda Pharmaceutical Company of Japan. It was approved by the US Food and Drug Administration (FDA) for the treatment of major depression in adults in September 2013. The structural formula of tioxetine is as follows: [0003] [0004] There are few synthetic methods of vortioxetine in the prior art. At present, the prior art process route is longer, the operation is cumbersome, the reaction time of some processes is long, the reaction conditions are high, and the solvent toxicity is large, which is unfavorable for suitability for industrialized production; The method of "cooking in one pot" has many by-products generated by side reactions during the reaction process, the produc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/096
CPCC07D295/096
Inventor 李沁沁王艳侨娄丽丽朱赞梅陈朋卫
Owner 郑州大明药物科技有限公司
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