反应详情

The product from step 1 (1.1 g, approx. 3.5 mmol) was dissolved in anhydrous CH2Cl2 (11 mL) and the solution was purged with N2, cooled in an ice bath, and treated with N-bromosuccinimide (0.498 g, 2.8 mmol). After stirring at 0–5° C. for one hour, the reaction mixture was partitioned between water (150 mL) and EtOAc (150 mL). The organic portion was washed with aqueous 5% NaHCO3 and brine, dried over MgSO4, filtered, and evaporated under vacuum to provide crude 7-(acetylamino)-4-bromo-9a-butyl-6-fluoro-1,2,9,9a-tetrahydro-3H-fluoren-3-one (1.35 g).

1. customthe solution was purged with N2
2. temperaturecooled in an ice bath
3. customthe reaction mixture was partitioned between water (150 mL) and EtOAc (150 mL)
4. washThe organic portion was washed with aqueous 5% NaHCO3 and brine
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. customevaporated under vacuum