反应详情

温度

90 °C

To a solution of 2-benzyl-7-(2-fluoroethyl)-7-(3-oxobutyl)-7,8-dihydrocyclopenta[e]indazol-6(2H)-one (10.8 g, 28.6 mmol) in 300 mL of toluene were added pyrrolidine (2.4 mL, 28.6 mmol) and acetic acid (1.64 mL, 28.6 mmol) and the solution was heated at 90° C. under nitrogen. After 15 hours, the solution was cooled to room temperature and partitioned between EtOAc and water. The organic phase was washed with 5% aqueous NaHCO3 and brine and dried over MgSO4. Evaporation of the solvent under vacuum gave a brown oil which was purified by chromatography on silica gel (1:2 to 1:1 EtOAc/hexanes) to give a sticky orange solid. The solid was dissolved in heptane-dichloromethane and then most of the dichloromethane was evaporated under reduced pressure. The resulting precipitated solid was isolated by filtration to give 2-benzyl-9a-(2-fluoroethyl)-8,9,9a,10-tetrahydroindeno[2,1-e]indazol-7(2H) -one.

1. temperaturethe solution was cooled to room temperature
2. custompartitioned between EtOAc and water
3. washThe organic phase was washed with 5% aqueous NaHCO3 and brine
4. dry with materialdried over MgSO4
5. customEvaporation of the solvent under vacuum
6. customgave a brown oil which
7. customwas purified by chromatography on silica gel (1:2 to 1:1 EtOAc/hexanes)
8. customto give a sticky orange solid
9. custommost of the dichloromethane was evaporated under reduced pressure
10. customThe resulting precipitated solid
11. customwas isolated by filtration