反应详情

温度

0 °C

To a solution of tert-butyl piperidin-4-ylcarbamate (200 g, 1 mol) and Et3N (150 g, 1.5 mol) in DCM (3000 mL) was added Ac2O (102 g, 1 mol) dropwise over 1 h, while maintained the temperature at 0° C. After addition, the mixture was stirred 0° C. for another 2 h, at which time TLC showed the reaction was completed. The solution was quenched by addition of water (1 L). The organic phase was collected and washed with saturated aqueous NaHCO3 (1 L), dried (Na2SO4) and concentrated to give crude product. Four batches were run in parallel and produced a combined crude product weight of 670 g. This crude was used directly in the step. LCMS (m/z): 243.1 (M+1).

1. additionAfter addition
2. customThe solution was quenched by addition of water (1 L)
3. customThe organic phase was collected
4. washwashed with saturated aqueous NaHCO3 (1 L)
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated
7. customto give crude product