4,4,5,5,6,6,7,7,8,8,9,9,9-tridecafluoronon-1-ene

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 10.7 g (25 mmol) of the Diels-Alder product of 4,4,5,5,6,6,7,7,8,8,9,9,9-tridecafluoro-1-nonene (perfluorohexyl-1-propene) and cyclopentadiene are mixed in 10 ml of dry toluene with 326 mg (1 mmol) of molybdenum acetylacetonate, and 13 ml of a2.9 molar solution of t-butyl hydroperoxide in toluene (37.5 mmol) are added dropwise at 22° C. within 30 minutes. During this period, thetemperature rises to 60° C. The solution is then held at 60° C. for another 2 hours. The low-boiling components are distilled off underreduced pressure at 40° C., and the residue is chromatographed on silica gel. The mobile solvent used is a mixture of hexane/methylene chloride/diethyl ether (10:10:0.5 parts by volume). The product-containingfractions are combined. After the mobile solvent is distilled off, 7.3 g ofa white solid remain behind. are added dropwise at 22° C. within 30 minutes During this period rises to 60° C The low-boiling components are distilled off underreduced pressure at 40° C. the residue is chromatographed on silica gel a mixture of hexane/methylene chloride/diethyl ether (10:10:0.5 parts by volume) After the mobile solvent is distilled off