反应详情

To the reaction solution of dimethyl 5,5′-[N-({6-amino-5-[(3-aminophenyl)ethynyl]pyridin-3-yl}carbonyl)sulfonimidoyl]dipentanoate (80 mg, 0.15 mmol, 1.0 equiv.), m-toluic acid (60 mg, 0.2 mmol, 1.3 equiv.), and DIPEA (0.11 mL, 0.6 mmol, 4.0 equiv.) in anhydrous DMF (1 mL) was added BOP (120 mg, 0.27 mmol, 1.8 equiv.) under nitrogen atmosphere. The reaction mixture was stirred at room temperature for overnight. It was then diluted with EtOAc, washed with sat. aq. NaHCO3, aq. NH4Cl, and brine, and finally dried with anhydrous Na2SO4. The solution was decanted, concentrated, and the oily residue was subject to a gradient column chromatography (from EtOAc-Hex 1:3 to 4:1) to afford the title compound as clear oil (76 mg). 1H NMR (DMSO-d6) δ: 10.29 (s, 1H), 8.57 (d, J=2.1 Hz, 1H), 8.07 (t, J=1.8 Hz, 1H), 8.04 (d, J=2.3 Hz, 1H), 7.79 (s, 1H), 7.74-7.78 (m, 2H), 7.38-7.46 (m, 4H), 7.00 (br. s., 2H), 3.54-3.63 (m, 10H), 2.41 (s, 3H), 2.39 (t, J=7.3 Hz, 4H), 1.71-1.86 (m, 4H), 1.64-1.71 (m, 4H)

1. washwashed with sat. aq. NaHCO3, aq. NH4Cl, and brine
2. dry with materialfinally dried with anhydrous Na2SO4
3. customThe solution was decanted
4. concentrationconcentrated