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By varying the proportions of the reactants antimony pentafluoride and xenon hexafluoride, it is possible to prepare each of the crystalline solids: XeF6·2SbF5, XeF6·SbF5, SbF5·2XeF6. Hydro

The invention relates to a synthetic method of octafluorocyclopentene, and belongs to the technical field of chemical engineering. The method comprises the following steps: dissolving perfluorocyclopentane, FeCp*2 and trifluoromethanesulfonate of alkali metal in a dry aprotic solvent, conducting stirring, conducting irradiating with a mercury lamp for 1-2 hours under the protection of protective gas to obtain a reaction product, and conducting separating and purifying to obtain octafluorocyclopentene. In the method, reactants react fully, operation is simple, reaction conditions are mild, hightemperature and high pressure are avoided, pollution discharge is easy after the reaction is finished, three wastes are few, aftertreatment is simple, the problem that many impurities are caused dueto the fact that fluorine-chlorine exchange cannot react fully is solved, the solvent can be recycled, pollution in the synthesis process is reduced, and the method is environmentally friendly and belongs to a green synthesis method.

Electrochemical fluorination (ECF) of the ester derivatives of oxolane-2-yl-carboxylic acid (1), oxolane-2-yl-methanol (2) and oxane-2-yl-methanol (3) were investigated. Perfluoro(oxolane-2-yl- carbonylfluoride) (4) was obtained from derivatives of 1 and 2, and perfluoro(oxane-2-yl-carbonylfluoride) (5) was obtained from derivatives of 3 as the desired compounds, respectively. From the ECF of acetates of 2 and 3, perfluorospiroethers having a dioxolane ring were also obtained as the cyclization product in low yield together with the desired perfluoroacid fluoride (4 and 5). The structure of these perfluorospiroethers was confirmed by analyzing the chlorinated products, which were obtained by the reaction with AlCl3.

Unlike alkyl bromides and iodides, alkyl chlorides are shown to be stable to direct fluorination, even under ultraviolett irradiation, at temperatures of 30 deg C and below.Although less reactive than the bromides and iodides, F-alkyl chlorides may be derivatized, presenting another example of direct fluorination-survivable functionality.High (63 percent) to moderate (32 percent) isolated yields of the analogous perfluororalkyl chlorides can be synthesized by aerosol direct fluorination of 1-chloropropane, 1-chlorobutane, 1-chloro-2-methylpropane, 1-chloro-3-methylbutane, 1-chlo-ro-2-methylbutane, and chlorocyclopentane with generally less than 20 percent C-C bond cleavage.Tertiary alkyl chlorides generally undergo intramolecular 1,2-chloride shift in the earliest stages of reaction in a manner characteristic of β-chloro radicals forming principally primary F-alkyl chlorides.Thus 2-chloro-2-methylpropane produces 1-chloro-F-2-methylpropane (47 percent), and 2-chloro-2-methylbutane produces a 16:6.3:1 ratio of 1-chloro-F-2-methylbutane, 1-chloro-F-3-methylbutane, and 2-chloro-F-3-methylbutane, respectively, in 32 percent combined yield.Secondary alkyl chlorides undergo a similar but incomplete rearrangement producing mixtures of primary and secondary F-alkyl chlorides.Thus 2-chloropropane produces a 2:1 mixture of 2-chloro-F-propane and 1-chloro-F-propane in 50 percent combined yield; 2-chlorobutane produces a 1:1.5 mixture of 2-chloro-F-butane and 1-chloro-F-butane in 34 percent combined yield, and 3-chloropentane produces a 2:3:1 mixture of 3-chloro-F-pentane, 2-chloro-F-pentane, and 1-chloro-F-pentane, respectively, in a combined yield of 30 percent.Because secondary alkyl chlorides partially rearrange but primary alkyl chlorides donot rearrange at all on fluorination, doubt is cast on the postulate that the intermediate radicals are equilibrating.