反应详情

To 890 mg (1.3 mmol) of crude 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-(4-fluoro-phenyl)-N-isopropyl-acetamide, prepared as in Intermediate 58, is added 10 mL of 4N HCl in dioxane at RT. The resulting solution is stirred 4 h and 100 mL of Et2O is added. The precipitate is filtered and purified by RP-HPLC (50-60% acetonitrile/ H2O over 30 min) to afford 86.7 mg of the title compound: 1H NMR (CDCl3, 300 MHz) δ7.85 (d, 1H, J=8.2), 7.43-7.09 (m, 15H), 6.96 (d, 1H, J=8.3), 5.01 (m, 1H), 4.98 (m, 2H), 3.82 (m, 2H), 1.05 (m, 6H); low resolution MS (FAB) m/e 576 (MH+); RP-HPLC Tr =5.5 min (40-60% acetonitrile/ H2O).

1. filtrationThe precipitate is filtered
2. custompurified by RP-HPLC (50-60% acetonitrile/ H2O over 30 min)