反应详情

Piperidin-4-one hydrochloride was added to a methanolic solution of sodium methoxide (prepared from anhydrous methanol (50 mL) and sodium metal (0.85 g, 37 mmol)) and heated at reflux for 2 h then concentrated to dryness in vacuo. The residue was dissolved in acetonitrile (100 mL), then potassium carbonate (10.22 g, 74 mmol) and 1-fluoro-4-nitro-benzene (3.92 mL, 37 mmol) were added and the mixture was heated at reflux overnight. The solvent was evaporated in vacuo, the residue being washed with water then 50% diethyl ether/petroleum ether and dried in vacuo to afford 1-(4-nitro-phenyl)-piperidin-4-one (3.01 g, 37%) as a yellow solid.

1. temperatureheated
2. temperatureat reflux for 2 h
3. concentrationthen concentrated to dryness in vacuo
4. dissolutionThe residue was dissolved in acetonitrile (100 mL)
5. temperaturethe mixture was heated
6. temperatureat reflux overnight
7. customThe solvent was evaporated in vacuo
8. washthe residue being washed with water
9. dry with material50% diethyl ether/petroleum ether and dried in vacuo