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

Participants

Reaction Conditions

Reaction Steps

98 g (1 mol) of cyclohexanone and 226 g (2 mol) of ethyl cyanoacetate were reacted with 204 g aqueous ammonia (equivalent to 3 mol of ammonia gas) in a solvent of methanol. After reacted at −5° C. to 0° C. for 24 hours, the reaction mixture was heated to 20 to 25° C. and stirred for 24 hours, and then heated to 60° C. Water is added in an amount equal to methanol, and the mixture was adjusted to pH 2-3 with sulfuric acid. The mixture was then cooled to below 5° C. and the precipitated 1,5-dicyano-2,4-dioxo-3-azaspiro[5,5]-undecane was collected by filtration.

Provenance & Evidence