反应详情

A stirred solution of 4-piperidinemethanol (1.72 g, 15.0 mmol) in acetone (100 ml) was added K2CO3 (4.14 g, 30. mmol) and 2,2,2-trichloroethyl 4-bromobutyrate (4.47 g, 15.0 mmol) and heated under reflux for 3 h. The reaction mixture was cooled to room temperature, filtered and the filtrate concentrated in vacuo. The residue was added CH2Cl2 (75 ml) and washed with brine (25 ml) and H2O (2×25 ml). The organic layer was dried over Na2SO4, filtered and evaporated in vacuo to leave the title compound as a viscous oil (4.70 g, 94.1%).

1. temperatureheated
2. temperatureunder reflux for 3 h
3. filtrationfiltered
4. concentrationthe filtrate concentrated in vacuo
5. additionThe residue was added CH2Cl2 (75 ml)
6. washwashed with brine (25 ml) and H2O (2×25 ml)
7. dry with materialThe organic layer was dried over Na2SO4
8. filtrationfiltered
9. customevaporated in vacuo