反应详情

Combine isopropyl-5-[acetyl-(3,5-bistrifluoromethylbenzyl)amino]-7-bromo-8-chloro-2,3,4,5-tetrahydrobenzo[b]azepine-1-carboxylate (0.050 g, 0.079 mmol), tris(dibenzylideneacetone)dipalladium (0) (0.0014 g, 0.0015 mmol), 2-di-tert-butylphosphino-2′,4′,6′-triisopropylbiphenyl (0.002 g, 0.0047 mmol), cesium carbonate (0.039 g, 0.119 mmol) and methanol (0.016 mL, 0.397 mmol) in toluene (1 mL) in a sealed tube and heat at 110° C. for 24 h. Dilute the cooled mixture with ethyl acetate (25 mL) and filter through Celite. Remove the filtrate solvent under reduced pressure and first purify the residue using chromatography on silica gel, eluting with hexanes/ethyl acetate (60:40), to provide the title compound as a white solid (0.017 g, 37%): ESI MS 581 (M+H).

1. filtrationfilter through Celite
2. customRemove the filtrate solvent under reduced pressure
3. customfirst purify the residue
4. washeluting with hexanes/ethyl acetate (60:40)