反应详情

温度

60 °C

To a solution of 5.9 g of tert-butyl (1-benzylpiperidin-4-yl)(2,3-dihydro-(1,4)dioxino(2,3-c)pyridin-7-yl methyl)carbamate in 30 mL of methanol, 1.2 g of 5% palladium carbon was added, and the mixture was stirred for 7 hours at 60° C. under a hydrogen atmosphere. The mixture was subjected to celite filtration, and 40 mL of ethyl acetate and 30 mL of a 0.5 mol/L sodium hydroxide aqueous solution were added to the filtrate. The organic layer was washed with saturated sodium chloride solution, dried using sodium sulfate and the solvent was evaporated under reduced pressure. The obtained residue was recrystallized from 5 mL of ethyl acetate-15 mL of heptane to give 3.0 g of tert-butyl ((2,3-dihydro-(1,4)dioxino(2,3-c)pyridin-7-yl)methyl)(piperidin-4-yl)carbamate monohydrate as a white powder.

1. filtrationThe mixture was subjected to celite filtration, and 40 mL of ethyl acetate and 30 mL of a 0.5 mol/L sodium hydroxide aqueous solution
2. additionwere added to the filtrate
3. washThe organic layer was washed with saturated sodium chloride solution
4. customdried
5. customthe solvent was evaporated under reduced pressure
6. customThe obtained residue was recrystallized from 5 mL of ethyl acetate-15 mL of heptane