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Cinepazide maleate crystal system and method for making same

A technology for crystallization of cinepazide maleate and cinepazide acid, which is applied in the direction of organic chemistry and can solve the problems that there are no research reports on the crystal form of cinepazide maleate

Inactive Publication Date: 2008-07-23
BEIJING SIHUAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, there is no research report on the crystal form of cinepazide maleate

Method used

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  • Cinepazide maleate crystal system and method for making same
  • Cinepazide maleate crystal system and method for making same
  • Cinepazide maleate crystal system and method for making same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Embodiment 1 Preparation of cinepazide maleate A crystal form one

[0046] In the dark, add cinepazide maleate (5g), add 25ml of anhydrous methanol, heat to dissolve the raw material, reflux for 5min, add dropwise to 150ml of vigorously stirred anhydrous ether within 30min, continue stirring for 2h after dripping, at room temperature After standing for 5 hours, the crystals were collected by filtration, and dried under high vacuum and reduced pressure at room temperature for 6 hours to obtain crystal form A of cinepazide maleate (4.5 g), with a melting point of 127-129° C. and an HPLC content of 99.6%.

Embodiment 2

[0047] Embodiment 2 Preparation of cinepazide maleate A crystal form two

[0048] Referring to the operation of Example 1, the solvent anhydrous ether was replaced with tetrahydrofuran (THF) to obtain cinepazide maleate A crystal form (3 g), with a melting point of 128-130° C. and a content of 99.4%.

Embodiment 3

[0049] Embodiment 3 Preparation of cinepazide maleate B crystal form one

[0050] In the dark, add cinepazide maleate (2g), add 40ml of anhydrous acetonitrile, heat to dissolve the raw material, reflux for 5min, cool at room temperature, filter and collect crystals after standing for 24h, dry under reduced pressure at room temperature for 10h, to obtain cinnamon maleate Pazide B crystal form (1.1g), melting point 170-172°C, content determined by HPLC method is 99.7%.

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Abstract

The invention relates to maleate cinepazide crystal forms and preparation methods, belonging to the medicine technical field, which comprises maleate cinepazide crystal form A, crystal form B, polymorphism containing crystal form B, and the preparation methods of the crystal forms.

Description

1. Technical field [0001] The invention belongs to the technical field of medicine, in particular to (E)-1-{4-[(3',4',5'-trimethoxycinnamoyl)]-1piperazine}acetylpyrrolidine maleate That is, the crystal form of cinepazide maleate and the preparation method thereof. 2. Background technology [0002] Cinepazide maleate is a known compound with the chemical name: (E)-1-{4-[(3',4',5'-trimethoxycinnamoyl)]-1piperazine}acetylpyrrole Pyridine maleate, the structural formula is as follows: [0003] [0004] Cinepazide maleate is a calcium ion channel blocker, by blocking Ca 2+ Transmembrane into vascular smooth muscle cells, so that vascular smooth muscle relaxation, cerebral blood vessels, coronary blood vessels and peripheral blood vessels to expand, thereby relieving vasospasm, reducing vascular resistance, increasing blood flow; enhancing the role of adenosine and cyclic adenosine monophosphate; improving red blood cell Flexibility and deformation can improve microcirculati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/18
Inventor 车冯升
Owner BEIJING SIHUAN PHARMA
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