Dehydrated crystalline form of 3Z 2 3 dihydro 3 4 methyl 2 4 methyl 1 piperazinyl acetyl amino phenyl amino phenylmethylene 2 oxo 1H indole 6 carboxylic acid methyl ester ethanesulfonate
Publication Date: 2015-Nov-11
The IP.com Prior Art Database
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Dehydrated crystalline form of (3Z)-2,3-dihydro-3-[[[4-[methyl[2-(4-methyl-1-piperazinyl) acetyl]amino]phenyl]amino]phenylmethylene]-2-oxo-1H-indole-6-carboxylic acid methyl ester ethanesulfonate
Described herein after is a dehydrated form of the hemihydrate form of (3Z)-2,3-dihydro-3- [[[4-[methyl[2-(4-methyl-1-piperazinyl) acetyl]amino]phenyl]amino]phenylmethylene]-2-oxo-1H- indole-6-carboxylic acid methyl ester ethansulfonate (referred to as Compound A).
The water content of the dehydrated form is of about 0.32%, (By KF) whereas the theoretical value of water content for Compound A as a hemihydrate form is 1.37%.
Figure 1: PXRD pattern of dehydrated Compound A:
Main PXRD peaks: 9.5, 9.9, 11.6, 13.7, 14.2, 16.4, 17.5, 18.9, 19.8, 20.1.
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.
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Water content determination - Karl Fischer (KF) method:
Water content determination of the p...