A method of preparing a monohalogenated nitroalkane which comprises reacting equal molar quantities of an alkali metal hydroxide and a nitroalkane in a suitable medium to form a nitronate salt therein, promptly mixing the medium containing the nitronate salt with an equal molar quantity of a halogen to form a monohalogenated nitroalkane in the medium, promptly adding a material to the medium containing the monohalogenated nitroalkane to terminate any further halogenation therein, and recovering the monohalogenated nitroalkane from the medium.