反应详情

Add 2 N hydrochloric acid (0.19 mL) to a solution of isopropyl 5-[acetyl-(3,5-bistrifluoromethylbenzyl)amino]-8-(benzhydrylideneamino)-2,3,4,5-tetrahydrobenzo[b]azepine-1-carboxylate (0.520 g, 0.747 mmol) in tetrahydrofuran (5 mL) at room temperature and stir for 3 h. Dilute the mixture with ethyl acetate (20 mL) and wash with saturated sodium bicarbonate solution and brine (10 mL each), then dry the organic layer over sodium sulfate, filter and remove the solvent under reduced pressure. Purify the residue using chromatography on silica gel, eluting with hexanes/ethyl acetate (1:1), to provide the title compound as an off-white solid (0.297 g, 75%): 530 (M−H).

1. washwash with saturated sodium bicarbonate solution and brine (10 mL each)
2. dry with materialdry the organic layer over sodium sulfate
3. filtrationfilter
4. customremove the solvent under reduced pressure
5. customPurify the residue
6. washeluting with hexanes/ethyl acetate (1:1)