Ammonia → 2,4-Dioxo-3-azaspiro(5.5)undecane-1,5-dicarbonitrile

Participants

Reaction Conditions

Reaction Steps

98 g (1 mol) of cyclohexanone and 282.5 g (2.5 mol) of ethyl cyanoacetate were reacted with 340 g aqueous ammonia (equivalent to 5 mol of ammonia gas) in a solvent of ethanol. After reacted at 5 to 10° C. for 24 hours, the mixture was heated to 25° C. and stirred for another 24 hours. The temperature was raised to 60° C. and water was added in an amount equivalent to the ethanol. The pH value was adjusted to 2 to 3 with sulfuric acid. The temperature was lowered to below 5° C. and the precipitated 1,5-dicyano-2,4-dioxo-3-azaspiro[5,5]-undecane was collected by filtration.

Provenance & Evidence