反应详情

温度

60 °C

To a stirred solution of tert-butyl(piperidin-4-ylmethyl)carbamate (22.3 g, 104 mmol) in methanol (120 mL) was added 1,6-dioxaspiro[2.5]octane (14.2 g, 124 mmol, prepared according to Satyamurthy, Nagichettiar et al., Phosphorus Sulfur, 1984, 19, 113) at room temperature. Then, the mixture was heated at 60° C. for 4 h. The volatile components were removed by evaporation and the resulting viscous oil was precipitated with a mixture of hexane and diethyl ether. The precipitate was collected by filtration and recrystallized from a mixture of n-hexane and 2-propanol to give the title compound 14.2 g (42%) as a colorless powder.

1. customThe volatile components were removed by evaporation
2. customthe resulting viscous oil was precipitated with a mixture of hexane and diethyl ether
3. filtrationThe precipitate was collected by filtration
4. customrecrystallized from a mixture of n-hexane and 2-propanol