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New Crystalline Forms of Idelalisib Hydrochloride

IP.com Disclosure Number: IPCOM000244272D
Publication Date: 2015-Nov-27
Document File: 6 page(s) / 48K

Publishing Venue

The IP.com Prior Art Database

Related People

Balazs Volk: AUTHOR [+2]

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New Crystalline Forms of Idelalisib Hydrochloride

Endréné Flórián, Ádám D. Detrich, Gyula Simig, Balázs Volk

Egis Pharmaceuticals Plc., Directorate of Drug Substance Development

P.O. Box 100, 1475 Budapest, Hungary

Idelalisib ((S)-2-(1-(9H-purin-6-ylamino)propyl)-5-fluoro-3-phenylquinazolin-4(3H)-one) is a drug used for the treatment of chronic lymphocytic leukemia. The substance acts as a phosphoinositide 3-kinase inhibitor.

Two new crystalline polymorphic forms of idelalisib HCl salt were isolated. New forms were prepared from acetonitrile medium and their crystal structures are characterized by their X-ray powder diffractogram.

X-ray powder diffraction measurements were carried out by applying the following conditions:

Instrument:                        PANalytical Empyrean X-ray powder diffractometer

Sample mode:                    Transmission

X-ray tube

Type:                                  Empyrean Long Fine Focus High Resolution tube

Anode material:                 Cu

Wavelength:                      Kα (1.541874 Å)

Focus mode:                      line focus

Incident beam optics

Divergence slit:                  Fixed slit 1/2 °

Mirror:                               Focusing elliptical mirror

Soller slit:                           0.04 rad

Anti-scatter slit:                 Fixed slit 1/2 °

Diffracted beam optics

Anti-scatter slit:                 Programmable slit in fix mode: 1/2 °

Soller slit:                           0.04 rad

Sample stage

Type:                                  Reflection-transmission spinner stage

Sample rotation:                1 rps

Beam knife:                       Transmission beam stop used

Detector                            

Type:                                  PIXcel 3D 1×1 area detector

Mode:                                Scanning line detector (1D) mode

Active length:                    3.3473°

Sample preparation:           place powder samples (without grinding) between two Mylar foils in the sample holder

Measurement settings

Temperature:                      room temperature

Accelerating voltage:         45 kV

Anode heating current:      40 mA

Scan type:                          continuous gonio (θ/θ) scan

Measurement range:          range: 2.0000 – 34.9964° 2θ

Step size:                           0.0131° 2θ

Time per step:                    109.650 s

Measurement cycles:         1

Measurement time:      ...