synthetic method | 4-piperidine ethanol (1.05g,8.13mmol) dissolve in dioxane/water (1: 1,50ml), then add Boc2O(2.13g,9.76mmol) and NaHCO3(8.62g,81.3mmol), the mixture was stirred at room temperature for 24h and then extracted with DCM. The mixed organic phases were washed successively with citric acid (N-Boc-4 solution) and aqueous NaHCO3 solution, followed by drying (Na2SO4), filtering and distilling the solvent to give 1, 4-piperidinethanol (1.77g,95%).. 1HNMR(CDCl3) Φ1.12 (dq,2h, J = 4.6Hz,11.8Hz),1.35-1.55(m,14h),2.70(t,2h, J = 12.8Hz),3.70(t,2h, J = 6.3Hz,-CH2CH2OH),3.95-4.20(m,2H);13C NMR(CDCl3) Δ28.7 (Boc-CH3),32.8,39.5,44.2,60.5,67.3,79.4(-C(CH3)3),155.1(C = O). |