反应详情

1-t-Butyl-4-piperidone (1.3 g, 8.4 mmol, 1.0 equiv), NaCN (0.61 g, 12.6 mmol, 1.5 equiv), and NH4Cl (0.67 g, 12.6 mmol, 1.5 equiv) were combined in 34 mL of 2 M NH3 in MeOH. The mixture was refluxed for 2 h at which time an additional 34 mL of 2 M NH3 in MeOH was added followed by another 2 h at reflux. The mixture was cooled and filtered. The filtrate was concentrated in vacuo and the residue was triturated with CH2Cl2 and filtered again. The solution was concentrated to a thick red oil which was used without further purification; MS, m/z 182=M+1.

1. additionwas added
2. temperatureat reflux
3. temperatureThe mixture was cooled
4. filtrationfiltered
5. concentrationThe filtrate was concentrated in vacuo
6. customthe residue was triturated with CH2Cl2
7. filtrationfiltered again
8. concentrationThe solution was concentrated to a thick red oil which
9. customwas used without further purification