Figure 2.54 and accompanying text.
The 1H NMR asssignment of the amino protons of 169 has been shown to be incorrect in the figure and as described in the text. A COSY spectrum demonstrated that the multiplet at –10.00 ppm can be assigned to the overlapping resonances of a single diasteeotopic proton of the NH2 group and the NHMe proton. The multiplet at –10.34 ppm is assigned to the other proton of the NH2 group.
Synthesis of 180. Add citation to H. Van Ryswyk, E. D. Turtle, R. Watson-Clark, T. A. Tanzer, T. K. Herman, P. Y. Chong, P. J. Waller, A. L. Taurog, C. E. Wagner, Langmuir, 1996, 12, 6143.