反应详情

温度

50 °C

To a solution of N-{2-[(8S)-2-methyl-2,6,7,8-tetrahydrocyclopenta[e]indazol-8-yl]ethyl}acetamide (80 mg, 0.311 mmol) in acetonitrile (3.1 mL) was added N-chlorosuccinimide (45.7 mg, 0.342 mmol), and the mixture was stirred at 50° C. for 5 hr. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (methanol/ethyl acetate=0/100→10/90), preparative HPLC (acetonitrile/water=10/90→90/10) and recrystallization (ethyl acetate/hexane) to give the title compound (20.1 mg, yield 22%).

1. customThe solvent was evaporated under reduced pressure
2. customthe residue was purified by silica gel column chromatography (methanol/ethyl acetate=0/100→10/90), preparative HPLC (acetonitrile/water=10/90→90/10) and recrystallization (ethyl acetate/hexane)