Acetic Acid → HCID 87172952, compound

Participants

Reaction Conditions

Reaction Steps

1.0 g of 1-methoxy-2,2,6,6-tetramethyl-4-cyano-4-trimethylsilyloxypiperidine is dissolved in 1.76 g acetic acid and 0.48 g acetone is added. 0.7 g conc. sulfuric acid is added and the reaction mixture is stirred at 70° C. for 18 h while forming a deep red solution. The reaction mixture is added to 40 ml saturated NaHCO3 solution, and extracted with 40 ml ethyl acetate. The organic phase is washed with H2O and subsequently dried over sodium sulfate. The solvent is removed in vacuo to leave 0.87 g of a tan residue. After washing the residue with n-hexane, 8-methoxy-2,2,7,7,9,9-hexamethyl-1-oxa-3,8-diaza-spiro[4.5]decan-4-one is obtained as a white solid (0.46 g), mp. 230° C.

Provenance & Evidence