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Crystalline pyrazoles

A crystal form and crystal technology, applied in the field of crystallized pyrazole derivatives, can solve problems that do not mention the separation and properties of the crystal form

Active Publication Date: 2011-08-10
ZOETIS SERVICE LLC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the preparation of the compound of formula I is disclosed, the specification does not mention its isolation and the nature of the crystalline form

Method used

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  • Crystalline pyrazoles
  • Crystalline pyrazoles
  • Crystalline pyrazoles

Examples

Experimental program
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Effect test

Embodiment 1

[0083] Mix 1 mL of deionized water and 1 mL of isopropanol thoroughly in a 20 mL glass vial. 4-[5-(4-Fluorophenyl)-3-(trifluoromethyl)-1H-pyrazol-1-yl]-benzenesulfonamide Form II (258.6 mg) was added to the vial. Place a magnetic stir bar and cap the vial tightly. The suspension was stirred for about 30 minutes at ~200 rpm. A thick pasty suspension was observed. Stirring was stopped and the vial was left to stand for 3 days. Remove a portion of the suspension and dry on absorbent paper. The powder X-ray pattern of the solid is shown at figure 1 middle. The melting point of some isolated crystals observed under a pyromicroscope was 148-152°C. However, this range was not reproducibly observed, as Form I transitions to Form II between 140 and 150 °C.

Embodiment 2

[0085] Suspend 380 mg of Form II in 2 mL of ethanol. Part of the compound dissolved while some excess solid compound was suspended in solution. The resulting suspension was stirred with a magnetic stir bar at a temperature of about 20°C to about 30°C for 2 weeks. At the end of this period, the solid was filtered and identified as Type I by PXRD.

Embodiment 3

[0087] 1.5 g of Form II was added to 2 mL of acetonitrile to form a suspension. The suspension was stirred with a magnetic stir bar at a temperature of about 20°C to about 30°C for 2 weeks. At the end of this period, the solid was filtered and identified as Type I by PXRD.

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Abstract

The present invention relates to crystal forms of 4-[5-(4-fluorophenyl)-3(trifluoromethyl)-1H-pyrazol-l-yl]-benzenesulfonamide and methods for preparation, interconversion, and isolation of such crystals.

Description

field of invention [0001] The present invention relates to the crystal form of 4-[5-(4-fluorophenyl)-3-(trifluoromethyl)-1H-pyrazol-1-yl]-benzenesulfonamide and the preparation, interconversion and Separation method. Background of the invention field of invention [0002] 5-Phenylpyrazolyl-1-benzenesulfonamides are a newly synthesized class of compounds with potent COX-2 inhibitory activity, which are useful in the treatment of arthritis and other conditions caused by inflammation. 4-[5-(4-Fluorophenyl)-3-(trifluoromethyl)-1H-pyrazol-1-yl]-benzenesulfonamide is 5-phenylpyrazolyl-1- Benzenesulfonamide: [0003] [0004] Formula I Background technique [0005] Compounds of formula I are disclosed in US Patent Nos. 5,466,823 (Tally et al.) and 5,521,207 (Graneto). These patents are incorporated herein by reference. Although the preparation of the compound of formula I is disclosed, the specification is silent on its isolation and the nature of the crystalline form. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D231/12A61K31/415A61P29/00H04W16/18H04W24/02
CPCC07D231/12H04W16/18H04W24/02A61P19/02A61P29/00A61P43/00
Inventor C·C·孙G·奥康纳
Owner ZOETIS SERVICE LLC