反应详情

In a hydrogenation apparatus 15 gm (0.06 mol) of nickel(II)acetate tetrahydrate, dissolved in 600 ml of 95% ethanol, were reduced in an atmosphere of hydrogen with 60 ml of a 1 M sodium borohydride solution, to yield black colloidal nickel boride (P-2-catalyst). In order to remove any unreacted borohydride, 14 gm (0.24 mol) of acetone were added, and the resulting mixture was shaken for 1 hour at room temperature and, after addition of 32.32 gm (0.123 mol) of (E)-4-(3-chloro-4-cyclohexyl-phenyl)-3-butene-2-one, it was hydrogenated at 5 atmospheres of hydrogen pressure until hydrogen absorption has ceased. The catalyst was filtered off, and the filtrate was concentrated by evaporation in vacuo. The residue shaken with a mixture of water and ethyl acetate, the organic phase was isolated, dried over sodium sulfate and evaporated, and the residue was distilled in vacuo. 19.0 Gm (58% of theory) of a colorless, viscous oil, b.p. 140°-148°C at 0.03 mm Hg were obtained.

1. additionwere added
2. customwas hydrogenated at 5 atmospheres of hydrogen pressure until hydrogen absorption
3. filtrationThe catalyst was filtered off
4. concentrationthe filtrate was concentrated by evaporation in vacuo
5. stirringThe residue shaken with a mixture of water and ethyl acetate
6. customthe organic phase was isolated
7. dry with materialdried over sodium sulfate
8. customevaporated
9. distillationthe residue was distilled in vacuo
10. custom19.0 Gm (58% of theory) of a colorless, viscous oil, b.p. 140°-148°C at 0.03 mm Hg were obtained