Abstract New bis (polyfluoroalkyl) diazomethanes have been obtained in high yield by the oxidation of polyfluorinated ketone hydrazones with bromine in water. A one-step preparative procedure for obtaining hexafluoroisopropylpentafluoroethylketone hydrazone from perfluoro-2-methyl-pent-2-ene and hydrazine hydrate has been worked out. Some reactions of the diazo compounds obtained, such as thermolysis, catalytic decomposition ...