International Journal of Analytical Chemistry / 2009 / Article / Tab 4

Research Article

A Multidisciplinary Investigation to Determine the Structure and Source of Dimeric Impurities in AMG 517 Drug Substance

Table 4

Partial and chemical shifts (δ /ppm) of the benzothiazole ring for AMG 517 and the enriched impurity fraction in DMSO-d6.

768743.tab.004

( /ppm, J/Hz) ( /ppm)

Position AMG 517 (a) Unknown 2 (b) Unknown 1 (b) AMG 517 (a) Unknown 2 (b) Unknown 1 (b)

16 7.35 (m, 1H) (c) 7.45 (d, 1H, J = 8.2 Hz) 7.59 (d, 1H, J = 8.0 Hz) 119.1120.4119.9
177.39 (t, 1H, J = 7.7 Hz) (c) 7.49 (d, 1H, J = 8.2 Hz)7.68 (d, 1H, J = 8.0 Hz)124.2128.1123.9
187.93 (m, 1H)119.6122.6131.2
19 133.6136.6132.8

(a) Data from 400 MHz NMR instrument; (b) data from 600 MHz instrument; (c) overlapping signals.

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