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Crystalline form of N-[4-[(3-Chloro-4-fluorophenyl)amino]-7-[[(3S)-tetrahydro-3-furanyl]oxy]-6-quinazolinyl]-4(dimethylamino)-2-butenamide

IP.com Disclosure Number: IPCOM000241005D
Publication Date: 2015-Mar-18
Document File: 3 page(s) / 495K

Publishing Venue

The IP.com Prior Art Database

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Crystalline form of N-[4-[(3-Chloro-4-fluorophenyl)amino]-7-[[(3S)-tetrahydro-3- furanyl]oxy]-6-quinazolinyl]-4(dimethylamino)-2-butenamide

Disclosed hereinafter is a crystalline form of N-[4-[(3-Chloro-4-fluorophenyl) amino]- 7-[[(3S)-tetrahydro-3-furanyl] oxy]-6-quinazolinyl]-4(dimethylamino)-2-butenamide (referred herein as compound I).

Figure 1: a powder XRPD pattern of crystalline compound I:

Intensity (counts)

8000

6000

4000

2000

0

5

10

15

20

25

30

35

2Theta (°)

XRPD peaks: 6.1, 11.0, 13.6, 14.1, 16.2, 17.1, 18.8, 20.2, 20.5 and 22.3 degrees two theta ± 0.2 degrees two theta.

Figure 2: a FTIR spectrum of crystalline compound I:


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X-Ray Power Diffraction:

After being powdered using mortar and pestle, samples were applied directly on a silicon plate holder. The X-ray powder diffraction pattern was measured with a Philips X'Pert PRO X-ray powder diffractometer, equipped with a Cu irradiation source =
1.54184 Ǻ (Ǻngström), X'Celerator (2.022º 2θ) detector. Scanning parameters: angle range: 3-40 deg., step size 0.0167, time per step 37 s, continuous scan. The accuracy of peak positions was defined as +/- 0.2 degrees due to experimental differences like instrumentations and sample preparations.

FTIR method :

Equipment

Instrument: Nicolet 6700 FT-IR spectrometer

Sample preparation: Sample was prepared as KBr pellet. Empty sample compartment was used for background spectrum acquisition.

Scanning parameters

The spectra were scanned between: 4000-40...