反应详情

温度

60 °C

A mixture of 4-(N-Boc-amino)-piperidine (1.0 g, 5.0 mmol), 2-hydroxybromopropane (1.0 g; 7.5 mmol) and TEA (0.76 g, 7.5 mmol) in AcCN (20 mL) was heated at 60° C. for 4 days. The reaction mixture was partitioned between EtOAc and water. The organic layer was separated, washed with brine, dried over Na2SO4 concentrated under reduced pressure. Purification of the residue by column chromatography on silica (0-5% 2M ammonia-MeOH in DCM) afforded [1-(2-hydroxy-propyl)-piperidin-4-yl]-carbamic acid tert-butyl ester (0.76 g, 59%) as an oil. LCMS (Method G; ESI): RT=0.49 min, m+1=259.3.

1. customThe reaction mixture was partitioned between EtOAc and water
2. customThe organic layer was separated
3. washwashed with brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated under reduced pressure
6. customPurification of the residue by column chromatography on silica (0-5% 2M ammonia-MeOH in DCM)