反应详情

Add a solution of cyanogen bromide (68 mg, 0.63 mmol) in ether (2.6 mL) to a solution of isopropyl 5-(3,5-bistrifluoromethyl-benzylamino)-8-chloro-2,3,4,5-tetrahydrobenzo[b]azepine-1-carboxylate (512 mg, 1.0 mmol) in ether (2.6 mL). Stir the mixture overnight at room temperature. Filter off the resulting solid and wash with ether. Wash the filtrate with water, dry over anhydrous sodium sulfate, filter and remove the solvent under reduced pressure. Purify the residue by flash chromatography, eluting with hexanes/ethyl acetate, to afford the title compound (204 mg, 38%): MS (ES+): 534 (M+H).

1. filtrationFilter off the resulting solid
2. washwash with ether
3. washWash the filtrate with water
4. dry with materialdry over anhydrous sodium sulfate
5. filtrationfilter
6. customremove the solvent under reduced pressure
7. customPurify the residue by flash chromatography
8. washeluting with hexanes/ethyl acetate