A method of preparing a nitrocarbonyl having at least 4 carbon atoms corresponding to the formula: ##EQU1## by contacting a dinitroalcohol having at least 5 carbon atoms corresponding to the formula: ##EQU2## with an alkaline agent at a temperature of from about 0.degree. to 200.degree.C. A valuable by product recoverable from the reaction is a nitroalkane. The contemplated nitrocarbonyls include nitroketones and nitroaldehydes which are useful as solvents, plasticizers, bactericides, lubricant additives and fuel additives.