反应详情

温度

80 °C

4-Benzyl-piperidine-4-carboxylic acid ethyl ester (2.5 g, 10 mmol), (2-bromo-ethyl)-carbamic acid benzyl ester (2.58 g, 10 mmol) and DIPEA (1.7 mL, 10 mmol) are dissolved in THF (50 mL) and heated at 80° C. for 15 h. The mixture is poured into Et2O (200 mL) and washed with sat. Na2CO3 (50 mL). The ether phase is extracted with 1M aqueous HCl (3×50 mL), the aqueous extracts washed with ether (50 mL) and adjusted to pH 14 with cooled 33% aqueous NaOH. The aqueous phase is extracted with CH2Cl2 (4×50 mL). The organic extracts are dried (Na2SO4), filtered and evaporated to provide the title compound.

1. washwashed with sat. Na2CO3 (50 mL)
2. extractionThe ether phase is extracted with 1M aqueous HCl (3×50 mL)
3. washthe aqueous extracts washed with ether (50 mL)
4. temperaturewith cooled 33% aqueous NaOH
5. extractionThe aqueous phase is extracted with CH2Cl2 (4×50 mL)
6. dry with materialThe organic extracts are dried (Na2SO4)
7. filtrationfiltered
8. customevaporated