Water → ST048623

Participants

Reaction Steps

15.2 g (0.046 mol) of 4-(cyclohexylcarbonyl)-2,6-dioxo-1-phenethyl piperazine are dissolved in 600 ml of ethanol. In an inert atmosphere, at 0° C., there are added 8.7 g (0.0509 mol) of dihydrated cupric chloride and the mixture is left for 1 hour at 0° C. To the reaction medium, kept at 0° C., are added in portions 8.8 g (0.23 mol) of sodium borohydride and left for 45 minutes at 0° C. The excess of reducing agent is destroyed by adding acetone. The insoluble salts are filtered and the filtrate is evaporated to dryness. The residue obtained is treated with a mixture of water and dichloromethane. The organic phase is decanted, dried over dry sodium sulphate and evaporated to dryness. The residue which is obtained is purified by filtration on a silica bed (elutrient: ethyl acetate). Beige crystals, m.p.=134° C., yield: 73%.

Provenance & Evidence