反应详情

26.7 g (0.18 mol) of 4-isobutylidenecyclohexanone (prepared with isobutyltriphenylphosphonium bromide/sodium hydride and cyclohexane-1,4-dione monoethylene ketal in DMSO, followed by hydrolysis of the ketal) in 200 ml of ammonia-saturated methanol was subjected to reductive amination at 100° C. at a hydrogen pressure of 100 bar in the presence of 6 g of Raney nickel. After the catalyst had been removed by filtration and the methanol had been stripped off, the crude product was distilled on a thin-layer evaporator (135° C./0.6 bar). 16.5 g (61% of theory) of a pale yellow oil were obtained.

1. customAfter the catalyst had been removed by filtration
2. distillationthe crude product was distilled on a thin-layer evaporator (135° C./0.6 bar)
3. custom16.5 g (61% of theory) of a pale yellow oil were obtained