反应详情

温度

60 °C

To a solution of (2R)-1-[3,5-bis(trifluoromethyl)-benzoyl]-2-(4-methoxybenzyl)-4-benzylpiperazine (4.90 g) in ethanol (50 ml) were added water (5 ml), ammonium formate (1.44 g), and 10% palladium on activated carbon [50% wet] (0.49 g) under nitrogen atmosphere. The reaction mixture was heated at 60° C. with stirring for 2 hours. Insoluble material was removed by filtration, and the filtrate was concentrated under reduced pressure. Ethyl acetate (40 ml) and water (40 ml) were added to the residue, and the organic layer was separated, washed with brine, and dried over magnesium sulfate. After removal of the solvent by evaporation, the resulting residue was purified by column chromatography on silica gel (70 g) using a mixed solvent of ethyl acetate and methanol (10:1). The fractions containing the objective compound were collected and evaporated under reduced pressure to give (2R)-1-[3,5-bis(trifluoromethyl)benzoyl]-2-(4-methoxybenzyl)piperazine (3.18 g) as syrup.

1. customInsoluble material was removed by filtration
2. concentrationthe filtrate was concentrated under reduced pressure
3. additionEthyl acetate (40 ml) and water (40 ml) were added to the residue
4. customthe organic layer was separated
5. washwashed with brine
6. dry with materialdried over magnesium sulfate
7. customAfter removal of the solvent
8. customby evaporation
9. customthe resulting residue was purified by column chromatography on silica gel (70 g)
10. additionThe fractions containing the objective compound
11. customwere collected
12. customevaporated under reduced pressure