CRYSTALLINE C21H22CL2N4O2 MALONATE

CRYSTALLINE C21H22CL2N4O2 MALONATE

A method of making Form A crystalline 4-(5-Chloro-2-isopropylaminopyridin-4-yl)-1H-pyrrole-2-carboxylic acid [1-(3-chlorophenyl)-2-hydroxyethyl]amide malonate having (i) an X-ray powder diffraction (XRPD) pattern comprising one or more peaks at 3.0 0.2, 5.2 0.2, 8.0 0.2, and 10.9 0.2 2e; and (ii) an...

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Hauptverfasser: DECRESCENZO, GARY, RIGSBEE, EMILY M, SELBO, JON G, WELSCH, DEAN, ALBERT, EKATERINA V
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creator DECRESCENZO, GARY
RIGSBEE, EMILY M
SELBO, JON G
WELSCH, DEAN
ALBERT, EKATERINA V
description A method of making Form A crystalline 4-(5-Chloro-2-isopropylaminopyridin-4-yl)-1H-pyrrole-2-carboxylic acid [1-(3-chlorophenyl)-2-hydroxyethyl]amide malonate having (i) an X-ray powder diffraction (XRPD) pattern comprising one or more peaks at 3.0 0.2, 5.2 0.2, 8.0 0.2, and 10.9 0.2 2e; and (ii) an infrared spectroscopy (IR) spectrum comprising one or more peaks at about 1573 2.0, 1504 2.0, 1475 2.0, 1253 2.0, 1033 2.0, and 883 2.0 cm-1, comprising the steps of: (a) suspending and stirring 4-(5-Chloro-2-isopropylaminopyridin-4-yl)-1H-pyrrole-2-carboxylic acid [1-(3-chlorophenyl)-2-hydroxyethyl]am ide free base in ethanol at ambient temperature to form a slurry; (b) adding 1.1 volume equivalents of malonic acid to the slurry and stirring at ambient temperature until solids of Form A malonate crystalline form; and (c) collecting the solids by vacuum filtration.
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