反应详情

To a solution of 9.83 g (0.55 mmol) of 2-benzyloxycarbonylamino-2-methyl-N-[2,3,4,5-tetrahydro-2-oxo-1-[[2'-[(t-butoxycarbonylamino)methyl][1,1'-biphenyl]-4-yl]methyl]-1H-benzazepin-3(R)-yl]propanamide (Step H) in 170 mL of methanol was added 120 mL of 9N aqueous hydrochloric acid. Periodically 10 mL portions of methanol were added to the reaction mixture to dissolve precipitates which form during the reaction (50 mL total). The reaction mixture was stirred overnight at room temperature then the solvent was removed under vacuum. The resulting oil was dissolved in methanol and the solvent was removed under vacuum to afford 8.57 g (96%) of the title compound as an off-white foam. 1H NMR (200 MHz, CD3OD): δ 1.40 (s, 6H), 1.90 (m, 1H), 2.20-2.65 (m, 3H), 4.02 (s, 2H), 4.32 (m, 1H), 4.96 (d, 16 Hz, 1H), 5.00 (s, 2H), 5.25(d, 16 Hz, 1H), 7.08-7.65 (m, 17H). FAB-MS: calculated for C36H38N4O4 590; found 591(M+H, 100%).

1. dissolutionto dissolve
2. customprecipitates which
3. customform during the reaction (50 mL total)
4. customthe solvent was removed under vacuum
5. dissolutionThe resulting oil was dissolved in methanol
6. customthe solvent was removed under vacuum