反应详情

Purge with nitrogen, a suspension of isopropyl-5-[acetyl-(3,5-bistrifluoromethylbenzyl)amino]-8-bromo-2,3,4,5-tetrahydrobenzo[b]azepine-1-carboxylate (0.153 g, 0.257 mmol), trimethylboroxine (36 μl, 0.257 mmol), and potassium carbonate (0.106 g, 0.771 mmol) in N,N-dimethylformamide (2 mL) in a 10 mL microwave vessel. Add tetrakis(triphenylphosphine)palladium (0) (0.030 g, 0.026 mmol) and irradiate the mixture at 150° C. for 20 min (50 W). Dilute the mixture with ethyl acetate (20 mL), wash with water and brine (10 mL each), then dry the organic layer over sodium sulfate, filter and remove the solvent under reduced pressure. Purify the residue first using chromatography on silica gel, eluting with hexanes/ethyl acetate (60:40), to provide the title compound as a white solid (0.056 g, 41%): 531 (M+H).

1. customPurge with nitrogen
2. washwash with water and brine (10 mL each)
3. dry with materialdry the organic layer over sodium sulfate
4. filtrationfilter
5. customremove the solvent under reduced pressure
6. customPurify the residue
7. washeluting with hexanes/ethyl acetate (60:40)