反应详情

200 mg of {1-(4-fluorophenyl)-3-[3-(4-fluorophenyl)-3-hydroxypropyl]-4-oxoazetidin-2-yl}-benzonitrile (16) were dissolved in 20 ml of ethanol and, with 0.5 ml of conc. ammonia, hydrogenated over Raney nickel at a hydrogen pressure of 75 bar and at 25° C. for 30 hours. The catalyst was filtered off with suction, the mixture was concentrated under reduced pressure and the residue was purified by column filtration (SiO2, CH2Cl2/methanol/conc. NH3=100:10:1). This gave the product of molecular weight 422.5 (C25H22F2N2O2); MS (DCI+): 423 (M+H+), 405 (M+H+-H2O).

1. filtrationThe catalyst was filtered off with suction
2. concentrationthe mixture was concentrated under reduced pressure
3. filtrationthe residue was purified by column filtration (SiO2, CH2Cl2/methanol/conc. NH3=100:10:1)
4. customThis gave the product of molecular weight 422.5 (C25H22F2N2O2)