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Preparation method of selexipag crystal form

A technology of Siripag and crystal form, which is applied in the field of medicine and can solve problems such as affecting product quality and easy residue of solvents

Inactive Publication Date: 2018-05-25
JIANGSU ALICORN PHARMATECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The corresponding preparation method is also mentioned in the patent. The solvent for preparing crystal form III is a high-boiling ester solvent such as n-butyl acetate, isopentyl acetate, and n-pentyl acetate. The solvent is easy to remain and affects product quality. Therefore, It is necessary to consider other crystallization solvents with low boiling point and easy removal when preparing crystal form III

Method used

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  • Preparation method of selexipag crystal form
  • Preparation method of selexipag crystal form

Examples

Experimental program
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Effect test

Embodiment 1

[0011] Embodiment 1: Preparation of cilipag crystal form

[0012] Add 5g of Silipag and 40ml of ethyl acetate into the reaction flask and continue to stir. The solution gradually dissolves at 75°C~80°C. After the dissolution, cool down to room temperature for crystallization. A large amount of white solids are precipitated in the reaction flask. Keep stirring at -5°C~5°C for 2 hours, filter to obtain a solid, and dry it at 40°C for 4 hours. The residual ethyl acetate is 0.086%, and the HPLC purity is 99.94%. The X-ray powder diffraction pattern is shown in Figure 1 Show:

[0013] The characteristic peaks are as follows:

[0014] 2θ(°)

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Abstract

The invention mainly aims at providing a preparation method of a selexipag crystal form. A diffraction pattern of X-ray powder of crystals prepared by utilizing the method has characteristic peaks at(2theta+ / -0.2 degrees) 9.3 degrees, 9.7 degrees, 16.8 degrees, 20.6 degrees and 23.5 degrees. The method has the advantages of simplicity in operation, less solvent residue, stable product quality andsuitability of industrialized mass production.

Description

technical field [0001] The invention belongs to the field of medicine, and the invention relates to a preparation method of cilipag crystal form. Background technique [0002] In claim 5 of the world patent WO2002088084, the chemical formula of Siripag is disclosed as 2-[4-[N-(5,6-diphenylpyrazin-2-yl)-N-isopropylamino] Butoxy}-N-(methylsulfonyl)acetamide, CAS accession number CAS is 475086-01-2, also known as NS-304, Siripag has excellent PGI2 receptor agonism, showing Platelet aggregation inhibition, vasodilation, bronchiectasis, lipid deposition inhibition, leukocyte activation inhibition and other pharmacological effects, the structure of Siripag is shown in formula (1): [0003] [0004] Formula 1) [0005] In the Chinese patent CN201080028176.8, three crystal forms of Siripag are disclosed, namely crystal form I, crystal form II and crystal form III. The corresponding preparation method is also mentioned in the patent. The solvent for preparing crystal form III i...

Claims

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Application Information

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IPC IPC(8): C07D241/20
CPCC07B2200/13C07D241/20
Inventor 刘玉先陆平波陈磊张逸
Owner JIANGSU ALICORN PHARMATECH CO LTD
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