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Acrylate esters of seven n‐1,1‐dihydroperfluoroalkanols have been synthesized. The esters are: 1,1‐dihydroperfluoroethyl‐; 1,1‐dihydroperfluoropropyl‐; 1,1‐dihydroperfluorobutyl‐; 1,1‐dihydroperfluoropentyl‐; 1,1‐dihydroperfluorohexyl‐; 1,1‐dihydroperfluorooctyl‐; and 1,1‐dihydroperfluorodecyl acrylates. Since these alcohols were difficult to esterify using conventional procedures, acrylyl chloride or acrylic acid plus perfluoroacetic anhydride have been empolyed in this work.

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Three distinct methods of preparation of 1, l-di-//-perfluoroalkyl halides have been developed in this laboratory. We wish to report a brief account of two of these methods along with the chemistry of some of the intermediates. The third method has been published (1).The first 1, l-di-JT-heptafluorobutyl halide ever prepared was 1,1-di-JTheptafiuorobutyl iodide. 1, l-Di-H-heptafiuorobutyl amine, C3F7CH2NH2, was reacted with nitrous acid in aqueous solution to give 1-17-hep tafiuorodiazobutane, C3F7CHN2, which was isolated by distillation in one run. Treatment of 1-7/heptafluorodiazobutane with an excess of hydrogen iodide in 3, d'-dichlorodiethyi ether at room temperature gave 1, l-di-H-heptafluorobutyl iodide, C3F7CH2L No reaction occurred at Dry Ice temperature, -78°.