反应详情

200 mg of 6 are 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 is filtered off with suction, the filtrate is concentrated under reduced pressure and the residue is purified by column filtration (SiO2, CH2Cl2/methanol/conc. NH3=100:10:1). This gives 7 of molecular weight 422.5 (C25H22F2N2O2); MS (DCl+): 423 (M+H+), 405 (M+H+—H2O).

1. filtrationThe catalyst is filtered off with suction
2. concentrationthe filtrate is concentrated under reduced pressure
3. filtrationthe residue is purified by column filtration (SiO2, CH2Cl2/methanol/conc. NH3=100:10:1)
4. customThis gives 7 of molecular weight 422.5 (C25H22F2N2O2)