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Iclaprim mesylate crystal form B and preparation method thereof

A technology of alaprime mesylate and crystal form, which is applied in the directions of sulfonate preparation, organic chemistry method, pharmaceutical formulation and the like, and achieves the effects of good stability and purity, low preparation cost and simple preparation method

Active Publication Date: 2020-02-21
SHANGHAI DUDE MEDICAL SCI & TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] CN200880129427.4 discloses the stability of eraprine mesylate aqueous solution. Under the condition of 20°C, the content drops from 99.1% to 97.5% in 45 days, which shows that there is stability of eraprine mesylate question

Method used

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  • Iclaprim mesylate crystal form B and preparation method thereof
  • Iclaprim mesylate crystal form B and preparation method thereof
  • Iclaprim mesylate crystal form B and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Suspend 5g of Ilaprim mesylate (HPLC purity: 98.8%) in 60ml of ethanol, under nitrogen protection, heat up to 80°C, add 0.5g of activated carbon after dissolving, stir for 10min, filter while hot, and the filtrate is at room temperature Crystals were precipitated under stirring for 1 hour, filtered, and dried to obtain 4.2 g of the solid, whose purity by HPLC was 99.7%.

Embodiment 2

[0037] Suspend 5g of Ilaprim mesylate (HPLC purity: 98.8%) in 70ml of isopropanol, under nitrogen protection, heat up to 90°C, then add 4ml of pure water until dissolved, then add 0.5g of activated carbon, and stir for 10min , filtered while hot, and the filtrate was stirred at room temperature to precipitate crystals for 1.5 hours, filtered, and 3.7 g of solids were dried, and the purity was 99.9% by HPLC.

Embodiment 3

[0039] Suspend 5g of Ilaprim mesylate (HPLC purity: 98.8%) in 60ml of methanol, under nitrogen protection, heat up to 70°C, add 0.5g of activated carbon after dissolving, stir for 10min, filter while hot, and the filtrate is at room temperature Crystals were precipitated under stirring for 1 hour, filtered, and 4.0 g of the solid was dried, and the purity was 99.8% by HPLC.

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Abstract

The invention provides a new crystal form B of iclaprim mesylate. An iclaprim mesylate crystalline solid B provided by the invention has the advantages of better stability, better purity and the like.In addition, the iclaprim mesylate crystalline solid B provided by the invention is simple in preparation method, low in preparation cost and suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of the crystal form of eraprine mesylate and a preparation method thereof. Background technique [0002] The structural formula of ICLAPRIM MESYLATE (ICLAPRIM MESYLATE) is shown in the following formula I. This compound can be used to control or prevent infectious diseases in mammals (human and non-human). In particular, it shows remarkable antibacterial activity even against multi-antibiotic Gram-positive strains and methicillin-resistant Staphylococcus aureus (MRSA). Typical combinations are, for example, sulfonamides or other enzyme inhibitors involved in folic acid biosynthesis, such as pteridine derivatives. The compound can also be co-administered with known antibacterial active substances, and exhibits synergistic effects on some of them. [0003] [0004] Polymorphism is an important property of compounds, and polymorphism generally exists for most chemical drugs. Different crystalline substanc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D405/06A61P31/04A61K31/506C07C309/04C07C303/32
CPCC07D405/06A61P31/04C07B2200/13Y02A50/30
Inventor 崔伟袁哲东魏艳
Owner SHANGHAI DUDE MEDICAL SCI & TECH CO LTD
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