反应详情

Carboxy benzene sulfonamide (20 μmol in 20 μL dry DMF (J. T. Baker), N-hydroxysuccinimide (22 μmol in 22 μL dry DMF), and EDC-HCl (14 μmol in 140 μL dry DMF) were mixed together and stirred at room temperature for 4 hours. The dipeptide H-leucine-glycine-OH (2 μmol in 20 μL dry DMF) and DIPEA (1.2 μL, 8 μmols) were added and the resulting mixture was stirred overnight at room temperature. ESI-MS calculated for [M−H+]−: 370.41 Found: 369.97. 1H NMR (DMSO-d6, 500 MHz) δ 8.72 (d, 1H, J=8.5 Hz), 8.30 (t, 1H, J=5.5 Hz), 8.09 (d, 2H, J=8 Hz), 7.94 (d, 2H, J=8 Hz), 7.52 (s, 2H), 4.61 (m, 1H), 3.77 (m, 2H), 1.72 (m, 2H), 1.62 (m, 1H), 0.95 (d, 3H, J=6.5 Hz), 0.92 (d, 3H, J=6.5 Hz). 13C NMR (DMSO-d6, 125 MHz) δ 173.0, 171.8, 166.0, 147.0, 137.7, 128.9, 126.2, 52.4, 41.5, 41.0, 25.1, 23.8, 22.0.

1. stirringthe resulting mixture was stirred overnight at room temperature