1,1,2,2,3,3,4-heptafluorocyclopentane

反応条件: temp:30.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Octafluorocyclopentane (at a purity of 99.9%, 42.4 g, 200 mmol) and 5% palladium carbon (2.12 g) were charged in a 70 ml-autoclave fitted with an agitator, for hydrogenation a hydrogen pressure of 6 kg/cm2 at 50° C. Fifteen hours later when hydrogen consumption was completely ceased, heating was terminated to stop the reaction. After sufficient neutralization with saturated sodium bicarbonate solution, the organic layer was separated, followed by addition of 200 ml of an aqueous sodium carbonate solution at a concentration of 1 mol. The resulting mixture was agitated at 30° C. for 10 hours. The reaction solution was separated into two layers; the resulting organic layer was again charged, together with 5% palladium carbon (1.78 g) and 1 g of tridecane, in a 70 ml-autoclave, for hydrogenation at 50° C. under a hydrogen pressure of 6 kg/cm2. When hydrogen absorption was ceased 15 hours later, the reaction was terminated in the same manner as described above; then, the resulting solution was neutralized with saturated sodium bicarbonate solution, followed by distillation, to recover 1,1,2,2,3,3,3,4-heptafluorocyclopentane (at a purity of 99.0%; 34.0 g). Fifteen hours later when hydrogen consumption heating was terminated the reaction After sufficient neutralization with saturated sodium bicarbonate solution, the organic layer was separated followed by addition of 200 ml of an aqueous sodium carbonate solution at a concentration of 1 mol The reaction solution was separated into two layers the resulting organic layer was again charged, together with 5% palladium carbon (1.78 g) and 1 g of tridecane, in a 70 ml-autoclave, for hydrogenation at 50° C. under a hydrogen pressure of 6 kg/cm2 When hydrogen absorption was ceased 15 hours later, the reaction was terminated in the same manner followed by distillation to recover 1,1,2,2,3,3,3,4-heptafluorocyclopentane (at a purity of 99.0%

反応条件: temp:30.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Octafluorocyclopentane (at a purity of 99.9%, 42.4 g, 200 mmol) and 5% palladium carbon (2.12 g) were charged in a 70 ml-autoclave fitted with an agitator, for hydrogenation a hydrogen pressure of 6 kg/cm2 at 50° C. Fifteen hours later when hydrogen consumption was completely ceased, heating was terminated to stop the reaction. After sufficient neutralization with saturated sodium bicarbonate solution, the organic layer was separated, followed by addition of 200 ml of an aqueous sodium carbonate solution at a concentration of 1 mol. The resulting mixture was agitated at 30° C. for 10 hours. The reaction solution was separated into two layers; the resulting organic layer was again charged, together with 5% palladium carbon (1.78 g) and 1 g of tridecane, in a 70 ml-autoclave, for hydrogenation at 50° C. under a hydrogen pressure of 6 kg/cm2. When hydrogen absorption was ceased 15 hours later, the reaction was terminated in the same manner as described above; then, the resulting solution was neutralized with saturated sodium bicarbonate solution, followed by distillation, to recover 1,1,2,2,3,3,3,4-heptafluorocyclopentane (at a purity of 99.0%; 34.0 g). Fifteen hours later when hydrogen consumption heating was terminated the reaction After sufficient neutralization with saturated sodium bicarbonate solution, the organic layer was separated followed by addition of 200 ml of an aqueous sodium carbonate solution at a concentration of 1 mol The reaction solution was separated into two layers the resulting organic layer was again charged, together with 5% palladium carbon (1.78 g) and 1 g of tridecane, in a 70 ml-autoclave, for hydrogenation at 50° C. under a hydrogen pressure of 6 kg/cm2 When hydrogen absorption was ceased 15 hours later, the reaction was terminated in the same manner followed by distillation to recover 1,1,2,2,3,3,3,4-heptafluorocyclopentane (at a purity of 99.0%

反応条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: One percent by weight of n-tridecane (dielectric constant 2.0), a low-polarity compound, was dissolved in crude 1,3,3,4,4,5,5-heptafluorocyclopentene having a purity of 99.9 GC %. An autoclave having a capacity of 100 ml was charged with a catalyst of activated carbon having supported thereon 5% by weight of powdered palladium. After the deaeration under reduced pressure, n-tridecane-containing 1,3,3,4,4,5,5-heptafluorocyclopentene prepared previously was poured. While the mixture was stirred at 40° C., the reaction was conducted by repeating block charge of hydrogen at a gauge pressure in the range of 0 to 6 kgf/cm2. After the completion of the reaction, the product was analyzed through gas chromatography. Consequently, a fluorinated saturated hydrocarbon containing 94 mol % of 1,1,2,2,3,3,4-heptafluorocyclopentane (HFCPA) and 6 mol % of 1,1,2,2,3,3-hexafluorocyclopentane was obtained. was charged with a catalyst of activated carbon having prepared previously was poured After the completion of the reaction

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

実験手順: To the 30 wt % 1,1,2,2,3,3,4-heptafluorocyclopentane solution of a perfluoropolyetherurethane acrylate composition, 0.06 g of butylhydroxytoluene was added, followed by dissolution while stirring. The resultant solution was warmed to 50° C. and 1,1,2,2,3,3,4-heptafluorocyclopentane was distilled off under reduced pressure (under about 100 mmHg for about 1.5 hours). 460 g of 2,2,3,3-tetrafluoropropanol was added and then distilled off under reduced pressure (under about 70 mmHg for about 2 hours) to obtain a 20 wt % 2,2,3,3-tetrafluoropropanol solution of a perfluoropolyetheracrylate composition (“20 wt % fluorine alcohol solution B of a perfluoropolyetherurethane acrylate composition”). followed by dissolution 1,1,2,2,3,3,4-heptafluorocyclopentane was distilled off under reduced pressure (under about 100 mmHg for about 1.5 hours) 460 g of 2,2,3,3-tetrafluoropropanol was added distilled off under reduced pressure (under about 70 mmHg for about 2 hours)

反応条件: temp:30.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Octafluorocyclopentane (at a purity of 99.9%, 42.4 g, 200 mmol) and 5% palladium carbon (2.12 g) were charged in a 70 ml-autoclave fitted with an agitator, for hydrogenation a hydrogen pressure of 6 kg/cm2 at 50° C. Fifteen hours later when hydrogen consumption was completely ceased, heating was terminated to stop the reaction. After sufficient neutralization with saturated sodium bicarbonate solution, the organic layer was separated, followed by addition of 200 ml of an aqueous sodium carbonate solution at a concentration of 1 mol. The resulting mixture was agitated at 30° C. for 10 hours. The reaction solution was separated into two layers; the resulting organic layer was again charged, together with 5% palladium carbon (1.78 g) and 1 g of tridecane, in a 70 ml-autoclave, for hydrogenation at 50° C. under a hydrogen pressure of 6 kg/cm2. When hydrogen absorption was ceased 15 hours later, the reaction was terminated in the same manner as described above; then, the resulting solution was neutralized with saturated sodium bicarbonate solution, followed by distillation, to recover 1,1,2,2,3,3,3,4-heptafluorocyclopentane (at a purity of 99.0%; 34.0 g). Fifteen hours later when hydrogen consumption heating was terminated the reaction After sufficient neutralization with saturated sodium bicarbonate solution, the organic layer was separated followed by addition of 200 ml of an aqueous sodium carbonate solution at a concentration of 1 mol The reaction solution was separated into two layers the resulting organic layer was again charged, together with 5% palladium carbon (1.78 g) and 1 g of tridecane, in a 70 ml-autoclave, for hydrogenation at 50° C. under a hydrogen pressure of 6 kg/cm2 When hydrogen absorption was ceased 15 hours later, the reaction was terminated in the same manner followed by distillation to recover 1,1,2,2,3,3,3,4-heptafluorocyclopentane (at a purity of 99.0%