反应详情

A suspension of rac-8-benzyl-4-phenyl-2,8-diaza-spiro[4.5]decan-1-one (28.8 g, 90 mmol) in MeOH: DCM (4: 1, 500 ml) was hydrogenated in the presence of Pd (10% on C, 14 g, 132 mmol) at 2 bar for 48 h at room temperature. After filtration over celite, the reaction mixture was evaporated and the residue dissolved in NaOH (2 N, 200 mnL). The product was extracted with DCM (3×150 mL) and the combined organic extracts dried over sodium sulfate. Filtration and evaporation afforded the title compound (13.1 g, 63%) as a white solid after trituration from diethylether. MS: m/e=231.4 (M+H).

1. filtrationAfter filtration over celite
2. customthe reaction mixture was evaporated
3. dissolutionthe residue dissolved in NaOH (2 N, 200 mnL)
4. extractionThe product was extracted with DCM (3×150 mL)
5. dry with materialthe combined organic extracts dried over sodium sulfate
6. filtrationFiltration and evaporation