Ammonium Chloride → HCID 66818142, compound

Participants

Reaction Conditions

Reaction Steps

LiOH.H2O (1.55 g, 36.9 mmol) was added to a solution of 4-carbamoyl-4-{[4-(3,3,3-trifluoro-propyl)-cyclohexanecarbonyl]-amino}-piperidine-1-carboxylic acid tert-butyl ester (5.53 g, 12.3 mmol) in ethanol (123 mL), and the mixture was stirred at 85° C. for two hours. A 50% saturated aqueous ammonium chloride solution was added to the reaction mixture, followed by extraction with ethyl acetate. The organic layer was then dried over MgSO4 and concentrated under reduced pressure. The resulting residue was purified by reprecipitation with hexane-ethyl acetate=3:1 to give 4-oxo-2-[4-(3,3,3-trifluoro-propyl)-cyclohexyl]-1,3,8-triaza-spiro[4.5]dec-1-ene-8-carboxylic acid tert-butyl ester (4.88 g, 92%).

Provenance & Evidence