International Journal of Analytical Chemistry / 2009 / Article / Tab 3

Research Article

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

Table 3

and chemical shifts (δ/ppm) of the enriched impurity fraction in DMSO-d6.

768743.tab.003

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

Position Unknown 2Unknown 1 Unknown 2 Unknown 1

1131.0 (q, = 31.7 Hz)131.0 (q, = 31.7 Hz)
2, 67.92 (d, 2H, J = 8.3 Hz)7.95 (d, 2H, J = 8.3 Hz)125.9125.9
3, 58.45 (d, 2H, J = 8.3 Hz)8.50 (d, 2H, J = 8.3 Hz)128.0128.0
4139.6139.6
7163.6163.5
98.81 (s, 1H)8.89 (s, 1H)158.5158.6 (b)
11170.1170.2
128.00 (s, 1H)8.11 (s, 1H)104.2104.4
13124.0 (q, = 273.2 Hz)124.0 (q, = 273.2 Hz)
15143.7143.5
167.45 (d, 1H, J = 8.2 Hz)7.59 (d, 1H, J = 8.0 Hz)120.4119.9
177.49 (d, 1H, J = 8.2 Hz)7.68 (d, 1H, J = 8.0 Hz)128.1123.9
18122.6131.2
19136.6132.8
20141.6141.9
22158.5158.4 (b)
2412.54 (s, 1H)12.55 (s, 1H)
25169.7169.7
262.12 (s, 3H)2.13 (s, 3H)22.522.6

(a) Signal splitting pattern: s = singlet, d = doublet, q = quartet; (b) interchangeable assignments.

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