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Crystalline form of 4-oxo-1,4-dihydroquinoline-3-carboxylic acid

IP.com Disclosure Number: IPCOM000227814D
Publication Date: 2013-May-20
Document File: 1 page(s) / 97K

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Crystalline form of 4-oxo-1,4-dihydroquinoline-3-carboxylic acid

Described herein below, is a crystalline form of 4-oxo-1,4-dihydroquinoline-3- carboxylic acid (referred to as compound B)

Experimental procedure:

Compound A (0.2 g) was slurried in water (7V vs. Compound A) followed by addition of 32% HCl (4.5V vs. Compound A). The resulting mixture was heated to 85 oC to give clear solution which was mixed at this temperature for 16h. The obtained precipitate was collected by suction filtration and the cake was washed till the filtrate reached pH=5-6. The obtained product was characterized by XRPD pattern. The XRD pattern is presented in the following representative X-ray diffractogram:

Sample ID: Analyst: Limor, Sample name: IVC IVC-5+Si., Temp: 25.0°C Date: 05/19/13 10:55 Step : 0.050° Integration Time: 1.000 sec

Range: 2.000 - 40.000° Cont. Scan Rate: 3.000 [°/min] Date: 05/12/13 12:14 Step : 0.050° Integration Time: 1.000 sec

Main XRD peaks of IVC-6 are: 8.7, 9.1, 13.4, 18.4, 20.1, 21.9, 22.5, 23.5, 26.3, 29.0,


31.1, 31.5, 36.0, 36.9 and 37.2 ± 0.2 degrees 2-theta.

The 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 rate of 3 deg/min. The peak at about 28.45° is attributed to silicon powder added as an internal standard.

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