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Preparing method for vortioxetine hydrobromide alpha crystal form

A technology of vortioxetine hydrobromide and hydrobromic acid, applied in the direction of organic chemistry and the like, can solve the problems of large particle size, high desolvation temperature, low purity of vortioxetine hydrobromide α crystal form and the like , to achieve the effect of high crystal purity, low desolvation temperature and suitable particle size

Active Publication Date: 2016-03-02
BEIJING BEILU PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The problem to be solved by the present invention is to provide a hydrogen bromide solution in order to solve the defects of high desolvation temperature and the low crystal form purity and large particle size of the obtained vortioxetine hydrobromide α crystal form in the existing method. A method for preparing vortioxetine α crystal form, the method has a low desolvation temperature, and the obtained vortioxetine hydrobromide α crystal form has high crystal purity, suitable particle size, and is suitable for industrial production

Method used

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  • Preparing method for vortioxetine hydrobromide alpha crystal form
  • Preparing method for vortioxetine hydrobromide alpha crystal form
  • Preparing method for vortioxetine hydrobromide alpha crystal form

Examples

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Embodiment 1 1

[0050] The preparation of embodiment 1-sec-butanol compound

[0051] Add 29g of vortioxetine hydrobromide and 524ml of sec-butanol into a 1L reaction flask, heat to 100°C and reflux for 30min, then lower the temperature at a rate of 0.2°C / min until it is cooled to room temperature, filter, and dry at 30°C for 2h. 27.2 g of white solid was obtained. Its X-diffraction, TGA, DSC atlas see Figure 1~3 , and its X-ray powder diffraction data are shown in Table 2.

[0052] X-ray powder diffraction expressed in 2θ angles figure 1 There are characteristic peaks at 6.61±0.2, 13.26±0.2, 15.98±0.2, 17.47±0.2, 19.17±0.2, 19.97±0.2 and 20.64±0.2.

[0053] its TGA figure 2 The thermal weight loss is about 15.11%, which is close to one molecule of sec-butanol, so it is a sec-butanol compound.

[0054] Its DSC image 3 Among them, there are endothermic peaks at 60.2°C, 103.0°C and 226.2°C.

Embodiment 2 1

[0055] The preparation of embodiment 2-sec-butanol compound

[0056] Heat 5 g of vortioxetine hydrobromide and 100 ml of sec-butanol to 100°C and reflux for 30 minutes, then lower the temperature at a rate of 0.5°C / min until cooled to room temperature, filter, and dry at 20°C for 2 hours to obtain 4.8 g of white solid .

Embodiment 3 1

[0057] The preparation of embodiment 3-sec-butanol compound

[0058] Heat 5 g of vortioxetine hydrobromide and 100 ml of sec-butanol to 100°C and reflux for 30 minutes, then lower the temperature at a rate of 0.1°C / min until it cools to room temperature, filter, and dry at 40°C for 2 hours to obtain 4.5 g of white solid .

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Abstract

The invention discloses a preparing method for a vortioxetine hydrobromide alpha crystal form. The preparing method comprises the following step that sec-butyl alcohol is removed from a vortioxetine hydrobromide-sec-butyl alcohol complex to obtain the vortioxetine hydrobromide alpha crystal form. The method is low in desolvation temperature, and the prepared vortioxetine hydrobromide alpha crystal form is high in purity, suitable in particle size and suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of vortioxetine hydrobromide alpha crystal form. Background technique [0002] [0003] Vortioxetine hydrobromide is developed by the Danish Lundbeck company, and its chemical name is 1-[2-(2,4-dimethyl-phenylthio)-phenyl]piperazine hydrobromide. The structure is shown in the formula 1. The compound has been approved by the US FDA for the treatment of major depressive disorder. Its mechanism may be to play an antidepressant effect by regulating 5-HT, and relevant pharmacological tests have found that the compound is 5-HT 3 , 5-HT 7 , 5-HT 1D Receptor antagonist, 5-HT 1B Partial agonists of receptors, 5-HT 1A receptor agonist. [0004] Vortioxetine hydrobromide exists in various crystal forms, and WO2007144005 reports several of its crystal forms, including: α, β, γ, hydrate, and ethyl acetate solvate. Among them, the melting point of the α crystal form is ~226°C, and the solubility in water is 2mg...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/096
CPCC07D295/096
Inventor 隋强吴茂诚刘帅唐超潘红娟刘晓慧董继鹏洪承杰
Owner BEIJING BEILU PHARM CO LTD
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