反应详情

N-Phenyl-4-piperidone (2.3 g, 13 mmol, 1.0 equiv) was dissolved in 26 mL of 2 M NH3 in MeOH and NaCN (0.76 g, 15 mmol, 1.2 equiv) and NH4Cl (0.80 g, 15 mmol, 1.2 equiv) were added and the mixture was refluxed for 2 h at which time an additional 26 mL of 2 M NH3/MeOH was added followed by another 2 h of reflux. The reaction mixture was cooled and filtered. The filtrate was concentrated. The crude product was purified by flash chromatography on SiO2 eluting with 100% CH2Cl2 and 2% MeOH in CH2Cl2 to give the pure product (1.92 g) as a thick yellow oil which solidified on standing; MS, m/z 202=M+1.

1. additionwas added
2. temperatureof reflux
3. temperatureThe reaction mixture was cooled
4. filtrationfiltered
5. concentrationThe filtrate was concentrated
6. customThe crude product was purified by flash chromatography on SiO2 eluting with 100% CH2Cl2 and 2% MeOH in CH2Cl2