Octafluorocyclopentane → 1H,1H,2H-Perfluorocyclopentane

Temperature

30 °C

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).

1. customFifteen hours later when hydrogen consumption
2. temperatureheating
3. customwas terminated
4. customthe reaction
5. customAfter sufficient neutralization with saturated sodium bicarbonate solution, the organic layer was separated
6. additionfollowed by addition of 200 ml of an aqueous sodium carbonate solution at a concentration of 1 mol
7. customThe reaction solution was separated into two layers
8. additionthe 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
9. customWhen hydrogen absorption
10. waitwas ceased 15 hours
11. customlater, the reaction was terminated in the same manner
12. distillationfollowed by distillation
13. customto recover 1,1,2,2,3,3,3,4-heptafluorocyclopentane (at a purity of 99.0%

ORD record

ord-bf4b494147a345678de97cb52854c819

Source dataset

uspto-grants-2001_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06312759B1