反应详情

Bromination of 1,1-dimethylethyl 7-hydroxy-8-nitro-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate (71 mg) was performed with NBS (41 mg) in DCM (2.2 ml) and SiO2 (426 mg) at −15° C. under nitrogen. After 15 minutes SiO2 was filtered off and the solvent was evaporated under reduced pressure. The crude was purified on silica gel (ethyl acetate/petroleum ether, 1/9) obtaining the title compound as a yellow solid (72 mg).

1. filtrationAfter 15 minutes SiO2 was filtered off
2. customthe solvent was evaporated under reduced pressure
3. customThe crude was purified on silica gel (ethyl acetate/petroleum ether, 1/9)