反应详情

温度

80 °C

1-tert-Butyl 4-methyl 4-(2-oxopropyl)piperidine-1,4-dicarboxylate (1.15 g, 3.84 mmol) in methanol (25 mL) was treated with ammonium acetate (3.85 g, 49.9 mmol), sodium cyanoborohydride (0.681 g, 10.83 mmol) and magnesium sulfate (2.54 g, 21.1 mmol). The mixture was heated at 80° C. in a sealed tube for 12 hours. The reaction mixture was filtered through a pad of CELITE® and the filter cake was washed with methanol. The filtrates were then concentrated and the residue was purified by column chromatography eluting with 0-10% methanol/ethyl acetate to afford the title compound. LC-MS (IE, m/z): 291.27 (M+23)+

1. filtrationThe reaction mixture was filtered through a pad of CELITE®
2. washthe filter cake was washed with methanol
3. concentrationThe filtrates were then concentrated
4. customthe residue was purified by column chromatography
5. washeluting with 0-10% methanol/ethyl acetate