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. Author manuscript; available in PMC: 2012 Feb 4.
Published in final edited form as: Org Lett. 2010 Dec 21;13(3):410–413. doi: 10.1021/ol1027199

Table 1.

NMR Assignments for EGM-556 (1) in DMSO-d6

structural
unit
position 13Ca δ, typeb 1H δ (m, J(Hz), int)c
Val-1 CO 168.7, qC
α 58.2, CH 4.24 (dd, 9.6, 6.0, 1H)
β 28.5, CH 2.25 (ds, 6.0, 6.6, 1H )
β-CH3 18.9, CH3 0.89 (d, 6.6, 3H)
β-CH3 19.3, CH3 0.89 (d, 6.6, 3H)
NH 7.60 (d, 9.6, 1H)
Ile-2 CO 170.4, qC
α 57.2, CH 4.26 (d, 9.6, 1H)
β 35.6, CH 2.05 (m, 1H)
γ 23.6, CH2 1.26 (m, 2H)
β-CH3 15.5, CH3 0.81 (d, 6.6, 3H)
γ-CH3 11.9 CH3 0.81 (t, 7.5, 3H)
NH 8.10 (d, 9.6, 1H)
Ala-3 CO 173.0, qC
α 48.8, CH 4.32 (dq, 6.3, 6.4, 1H)
α-CH3 16.3, CH3 1.18 (d, 7.2, 3H)
NH 8.56 (d, 6.3, 1H)
Val-4 CO 172.3, qC
α 57.5, CH 4.14 (dd, 8.7, 7.2, 1H)
β 29.8, CH 1.96 (ds, 6.9, 6.8, 1H)
β-CH3 19.6, CH3 0.89 (d, 6.6, 3H)
β-CH3 18.2, CH3 0.89 (d, 6.6, 3H)
NH 7.74 (d, 8.7, 1H)
Hyppa-5 1 168.7, qC
2 40.1, CH2* 2.42 (dd. 14.4, 1.8, 1H)
2.88 (dd, 14.4, 10.5, 1H)
3 72.9, CH 5.50 (ddd, 10.5, 7.1, 1.8, 1H)
4 126.7, CH 6.28 (dd, 15.9, 7.1, 1H)
5 132.4, CH 6.68 (d, 15.9, 1H)
6 135.7, qC
7 126.5, CH 7.44 (d, 7.2, 2H)
8 128.7, CH 7.36 (dd, 7.5, 7.2, 2H)
9 128.1, CH 7.28 (t, 7.5, 1H)
a

Measured at 150 MHz.

b

Carbon type established from 13C DEPT and/or gHMQC experiments.

c

Measured at 600 MHz.

*

Overlapping with DMSO-d6