Crystal form of fumarate of pyrrole derivative

A fumarate and crystallization technology, applied in the direction of organic chemistry, etc., to achieve the effect of high purity and good stability

Inactive Publication Date: 2015-02-04
SUNCADIA PHARM CO LTD +1
View PDF1 Cites 16 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] CN101300229A discloses 1-[5-(2-fluorophenyl)-1-(pyridin-3-ylsulfonyl)-1H-pyrr

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Crystal form of fumarate of pyrrole derivative
  • Crystal form of fumarate of pyrrole derivative
  • Crystal form of fumarate of pyrrole derivative

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0041] Example 1

[0042] The preparation method of pyrrole derivative maleate with crystal form A is described in detail below.

[0043] Step 1: Synthesis of 5-(2-fluorophenyl)-1-(pyridine-3-sulfonyl)-1H-pyrrole-3-carbaldehyde

[0044] Compound II (260 mg) was dissolved in tetrahydrofuran (50 ml), 60% NaH was added, and the reaction was stirred at room temperature for 30 minutes. Then add 15-crown ether-5 (1.5g), stir and react at room temperature for 1 hour, then add pyridine-3-sulfonyl chloride, stir and react at room temperature for 2 hours until TLC traces the reaction to completion, then add 20 mL of saturated brine to the reaction system , Extracted with ethyl acetate (100 mL×2), combined the organic phases, washed the organic phases with 50 ml of saturated brine, dried an appropriate amount of anhydrous sodium sulfate, filtered, and concentrated the filtrate under reduced pressure to obtain the crude compound IV (200 mg) directly into the next reaction.

[0045] Step 2: Synth...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention relates to a crystal form of fumarate of a pyrrole derivative, and concretely relates to a crystal form of 1-[5-(2-fluorophenyl)-1-(prindine-3-ylsulfonyl)-1H-pyrrol-3-yl]-N-methylmethamide monofumarate and a preparation method thereof. An X-ray powder diffraction spectrum represented by 2theta angle and the interplanar distance by performing Cu-Ka radiation on the crystal form, and is shown as figure 1. The crystal form is high in purity and good in stability, is applicable to preparation technological process and long-term storage, and also has superiority in industrialized production.

Description

technical field [0001] The present invention relates to a kind of 1-[5-(2-fluorophenyl)-1-(pyridin-3-ylsulfonyl)-1H-pyrrol-3 base]-N-methylmethylamine monofumarate Crystalline forms and methods for their preparation. Background technique [0002] In the development of pharmaceutical compositions, it is very important that the drug is in a form that can be easily handled and processed. In manufacturing, it is also very important to be able to provide the drug in the purest possible crystalline form. It would be desirable if an active pharmaceutical ingredient could be easily obtained in a stable crystalline form. Therefore, in producing commercially viable and pharmaceutically acceptable pharmaceutical compositions, whenever possible, the drug should be provided in a substantially crystalline and stable crystalline form. [0003] 1-[5-(2-Fluorophenyl)-1-(pyridin-3-ylsulfonyl)-1H-pyrrol-3yl]-N-methylmethylamine monofumarate was developed by Takeda Pharmaceutical Company A g...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07D401/12
CPCC07D401/12
Inventor 孙飘扬吕小虎吴成龙孙绍光黄金昆张羽
Owner SUNCADIA PHARM CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap