1-Methyl-4-piperidone → HCID 54060679, compound

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Reaction Steps

1-Methyl-4-piperidone (0.47 g, Aldrich) was added to a stirred solution of the product from step (b) (0.30 g) in glac. acetic acid (2.0 ml) and the mixture stirred at 100° C. for 2 hours. The cooled mixture was poured onto ice/NH4OH (20 ml) and the resulting solid filtered off. The latter was eluted through a silica column using DCM/EtOH/NH4OH (60:8:1) as eluant and crystallised from ethyl acetate to give the desired product as a colourless solid (0.11 g), mp 225°-227° C., [α]D20 -45.4° (c=0.5, IN aqu. HCl). Elemental analysis and 1H NMR were consistent with the proposed structure.

Provenance & Evidence