Reaction Steps
(3R,5S,8S)-22-ethyl-8-isopropyl-7-oxo-2,27-dioxa-6,9,11,12,24-pentaazapentacyclo[16.6.2.13,6.110,13.021,25]octacosa-1(24),10,12,18,20,22,25-heptaene-5-carboxylic acid (from Step 3) was dissolved in DMF and to this solution was added Intermediate 2 followed by iPr2NEt (3.5 eq) and TBTU (1.09 eq). The resulting reaction mixture was stirred 12 h at RT and purified by reverse phase HPLC to give the title compound as a white solid. 1H NMR (600 MHz, DMSO-d6) δ 10.33 (s, 1H), 8.92 (s, 1H), 7.96 (d, J 9.7, 1H), 7.87 (d, J 8.6, 1H), 7.78 (s, 1H), 7.71 (s, 1H), 7.63 (dd, J 8.6, 1.5, 1H), 5.71 (s, 1H), 5.59 (m, 1H), 5.20 (d, J 17.2, 1H), 5.08 (d, J 10.2, 1H), 4.88 (d, J 10.8, 1H), 4.20 (dd, J 11.3, 7.2, 1H), 4.17 (t, J 9.6, 1H), 3.96 (dd, J 11.4, 3.4, 1H), 2.94-2.86 (m, 4H), 2.76 (m, 1H), 2.64 (m, 1H), 2.18-2.09 (m, 3H), 1.75-1.69 (m, 3H), 1.67-1.62 (m, 2H), 1.39-1.36 (m, 2H), 1.29-1.24 (m, 4H), 1.10-1.08 (m, 2H), 1.04-1.03 (m, 2H), 1.00 (t, J 6.6, 3H), 0.96 (d, J 6.6, 3H). MS (ES+) C36H45N7O7S requires: 719. Found: 720 (M+H+).
