反应详情

400 mg of 2-[3-(1-tert-butoxycarbonyl-1H-indazol-3-ylmethyl)-2,4-dioxo-5-phenyl-2,3,4,5-tetrahydro-benzo[b][1,4]diazepin-1-yl]-N-isopropyl-N-phenyl-acetamide, prepared as in Intermediate 68, is dissolved in 10 mL of CHCl3 and 5 mL of TFA is added. The reaction mixture is stirred for 6 h and the solvents were removed in vacuo and the residue is purified by flash column chromatography on silica gel (MeOH 1%:CHCl3 99%) to afford 240 mg of the title compound: 1H NMR (400 MHz, CDCl3) δ7.93 (d, 1H, J=8.4), 7.51-7.19 (m, 16H), 6.99 (m, 1H), 5.03 (m,1H, J=6.8), 4.29 (d, 1, J=16.4), 4.26 (d, 1H, J=16.4), 4.14 (m, 1H), 3.89 (dd, 1H, J=16.5, 6.4), 3.82 (dd 1H,J=16.5, 6.4,), 1.08 (t, 6H, J=6.8); LOW RESOLUTION MS (FAB) m/e 558 (MH+); Tr =9.90 min. (HPLC Column: Dynamax C-8 2 mL/min., 50-90% Acetonitrile in aqueous TFA (0.1% v/v) over 15 min.).

1. customthe solvents were removed in vacuo
2. customthe residue is purified by flash column chromatography on silica gel (MeOH 1%:CHCl3 99%)