Nitrozation of ω-substituted alkanoic acids of the general formula X(CH2) nCO2H (X = CI, CO2H, CO2Me, PhthN), bulky substituted alkanoic acids, arylacetic acids containing electron withdrawing substituents in the aromatic ring, o-tosylhydroxyphenylacetic acids and N-phtaloilaminophenylacetic acids yield nitriles with the carbon chain shortened by one (or two for dicarboxylic acids) carbon atom.