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Crystalline Forms of CAS 77883-43-3 Intermediates

IP.com Disclosure Number: IPCOM000228596D
Publication Date: 2013-Jun-20

Publishing Venue

The IP.com Prior Art Database

Abstract

Crystalline intermediates for Pfizer active pharmaceutical ingredient 77883-43-3 were characterized using Powder X-ray Diffraction and Differential Scanning Calorimetry.

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Pfizer Inc

235 East 42nd Street

New York

,

NY

10017-5755

 
 
 
 
 
 

Title:  Crystalline Forms of CAS 77883-43-3 Intermediates

                                                                                                                

Authors:  Christina Pattoni, Nicholas J. Lawson, Dennis J. Stelzer

Abstract: Crystalline intermediates for Pfizer active pharmaceutical ingredient 77883-43-3 were characterized using Powder X-ray Diffraction and Differential Scanning Calorimetry.

Summary:  Intermediates of active pharmaceutical ingredients often occur in crystalline form.  Crystallinity affords advantages of stability of the intermediate and of purification of the intermediate.  Three intermediates of 77883-43-3 active pharmaceutical ingredient were characterized using Powder X-ray Diffraction and Differential Scanning Calorimetry.

Experimental: 

Powder X-Ray Diffraction (PXRD)

Powder X-ray diffraction was performed using a Scintag X1 Advanced Diffraction System operating under Scintag DMS/NT™ 1.36b and Microsoft Windows 2000 software.  The systems use a copper X-ray source maintained at 45 kV and 40 mA to provide Cu KL3 (Ka1) emission of 1.5406 Å and a solid state peltier cooled detector.  Beam aperture was controlled using tube divergence and anti-scatter slits of 2 and 4 mm and detector anti-scatter and receiving slits of 0.5 and 0.3 mm width.  Data were collected using a step scan of 0.03°/point with a one second/point counting time over a range of 2 to 40° two-theta.  Scintag Round, Top Loading stainless steel Sample Cups were utilized for all analyses.  Samples were run using the full cup volume when enough material was provided.  Otherwise, 12 mm or 9 mm aluminum tray inserts were used to accommodate small sample volumes.  Samples were either run without treatment (as is) or after being hand ground (h.g.) using a mortar and pestle just prior to analysis.  Data analysis and graphic output were generated using JADE Materials Data software from Materials Data Incorporated.  Peaks were identified using a Quartic filter algorithm with a threshold (ESD) of 3.0, an intensity cutoff of 0.5%, and averaging over seven points.

Differential Scanning Calorimetry (DSC)

DSC was performed using a TA Instruments model 2920 module with a Thermal Analyst 5000 controller. Samples of about 1 to 2 mg were accurately weighed into aluminum pans with lids that were crimped to ensure good thermal contact and provide an hermetic seal. The samples were evaluated using a linear heating ramp of 5 °C/min from ambient to approximately 300°C. The cell was purged with a dry nitrogen flow of 40 sccm. Data were collected using Thermal Advantage 4.2.1 software and analyzed using Universal Analysis V4.2E.

Results:  Table 1 summarizes the compounds that were characterized and which analytical technique was used.  The chemical name as well as the Chemi...