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Crystalline ethyl 1-(4-methoxyphenyl)-6-(4-nitrophenyl)-7-oxo-4,5,6,7-tetrahydro-1H-pyrazolo[3,4-c]pyridine-3-carboxylate

IP.com Disclosure Number: IPCOM000233229D
Publication Date: 2013-Dec-03
Document File: 3 page(s) / 105K

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The IP.com Prior Art Database

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Crystalline ethyl 1-(4-methoxyphenyl)-6-(4-nitrophenyl)-7-oxo- 4,5,6,7-tetrahydro-1H-pyrazolo[3,4-c]pyridine-3-carboxylate

Disclosed herein is a crystalline form of ethyl 1-(4-methoxyphenyl)-6-(4- nitrophenyl)-7-oxo-4,5,6,7-tetrahydro-1H-pyrazolo[3,4-c]pyridine-3-carboxylate ("compound I").

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

Sample ID: Analyst:uri, Sample name: APX SY-17167, Temp: 25.0°C Date: 11/28/13 08:20 Step : 0.050° Integration Time: 1.000 sec

Range: 2.000 - 40.000° Cont. Scan Rate: 3.000 [°/min] Vert. Scale Unit: [CPS] Horz. Scale Unit: [deg]

Date: 11/26/13 09:54 Step : 0.050° Integration Time: 1.000 sec

20000

16000

CPS

12000

8000

4000

0


2.0


6.0


10.0 14.0 18.0 22.0 26.0 30.0 34.0 38.0

degrees 2-theta

XRPD peaks: 3.8, 7.6, 8.4, 10.7, 13.6, 15.0, 15.5, 16.9, 18.8, 19.9, 20.4, 21.8,


22.9, 23.9, 24.2, 25.7, 26.3, 27.3 and 29.6 ± 0.2 degrees 2-theta.


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Figure 2: a FTIR spectrum of crystalline compound I:


2.8


2.6


2.4


2.2


2.0


1.8


1.6


1.4

K-M


1.2


1.0


0.8


0.6


0.4


0.2


0.0

-0.1

4000

3500

3000

2500

2000

1500

1000

500

400

cm-1

Name

Description

Apixaban SY-17167

28 11 2013 Drift KBr; 4000-400cm-1; 16 scans; resolution:4.0cm-1; analyst: Motti

X-Ray Power Diffraction:

XRPD analysis was performed on ARL (SCINTAG) powder X-Ray diffractometer model X'TRA equipped with a solid state detector. Copper radiation of 1.5418 Å was used. Scanning parameters: range: 2-40 degrees two-theta; scan mode: continuous scan; step size: 0.05°.; and a...