1,1,1,4,4,4-hexafluorobutane

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: 40 g (0.2 mol) of 1,1,1,4,4,4-hexafluoro-2-chloro-2-butene were hydrogenated in 300 ml of ethanol in the presence of 12 g of potassium hydroxide and 24 g of Raney nickel in the pressure range of from 20 to 40 bar and at a temperature from 20 to 100° C. The solid components were filtered off, the solvent was extracted with water, and the organic phase was separated and purified by distillation to give 15.5 g (47% of theory) of 1,1,1,4,4,4-hexafluorobutane. The boiling point was 25 to 27° C. at 1013 mbar. The solid components were filtered off the solvent was extracted with water the organic phase was separated purified by distillation

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

実験手順: In a stainless steel autoclave, 40 g of 1,1,1,4,4,4-hexafluoro-2-chloro-2-butene in 300 ml of ethanol were hydrogenated with hydrogen in the presence of 12 g of potassium hydroxide and 25 g of Raney nickel for 3 hours at 20° C. and another 1 hour at 100° C. at a pressure of from 30 to 40 bar. The solid components were then removed from the reaction mixture by filtration and the remaining liquid was distilled to give 16 g of 1,1,1,4,4,4-hexafluorobutane having a boiling point of 25-30° C. at 1013 mbar. The mass spectrum showed a molecular ion at m/e 166. The solid components were then removed from the reaction mixture by filtration the remaining liquid was distilled

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: To 1,1,1,4,4,4-hexafluoro-2,3-dichloro-2-butene (23.5 g, 0.1 mole) in 50 ml tetrahydrofuran were added sodium hydroxide (8.5 g) and as catalyst 5% by weight palladium on carbon (3 g). This mixture was hydrogenated with hydrogen at temperatures of 20 to 40° C. under pressures of 20 to 40 bar. The reaction mixture was worked up as in Example B, producing 8.0 g (75% of theory) of 1,1,1,4,4,4-hexafluorobutane.

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

実験手順: 1,1,1,4,4,4-Hexafluoro-2-chloro-2-butene in 300 ml ethanol was hydrogenated in the presence of potassium hydroxide (12 g) and Raney nickel (25 g) at a temperature of 20° to 100° C. and under a pressure of 20 to 40 bar. The solid constituents were filtered off and the filtrate was extracted with water. The organic phase was separated and purified by distillation, giving 15.5 g (47% of theory) of 1,1,1,4,4,4-hexafluorobutane, boiling point 24°-27° C. at 1013 bar. The solid constituents were filtered off the filtrate was extracted with water The organic phase was separated purified by distillation

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

実験手順: 1,1,1,4,4,4-Hexafluoro-2-bromo-3-chloro-2-butene (10 g, 36 mmole) in 50 ml tetrahydrofuran was hydrogenated in the presence of sodium hydroxide (3.0 g) and Raney nickel (5 g) at a temperature of 20° to 40° C. and under a hydrogen pressure of 20 to 40 bar. The reaction mixture was worked up as in Example B, producing 3.5 g (59% of theory) of 1,1,1,4,4,4-hexafluorobutane.

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

実験手順: 1,1,1,4,4,4-Hexafluoro-2-chloro-2-butene (199 g, 1 mole) in 800 ml diglyme was hydrogenated in the presence of sodium hydroxide (45 g) and Raney nickel (30 g) at a temperature of 20° to 40° C. and under a pressure of 20 to 40 bar. The solid constituents were filtered off and the filtrate was extracted with water. The organic phase was separated and purified by fractional distillation, giving 125 g (75% of theory) of 1,1,1,4,4,4-hexafluorobutane, boiling point 24°-27° C. at 1013 mbar. The 19F-nmr spectrum showed a resonance at -10.7 ppm (standard: CF3CO2H). The solid constituents were filtered off the filtrate was extracted with water The organic phase was separated purified by fractional distillation

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

実験手順: 1,1,1,4,4,4-Hexafluoro-2-chloro-2-butene (40 g) (prepared according to the method described by J. H. Babcock et al in Preparation, Properties, and Technology of Fluorine and Organic Flyoro Compounds, eds. C. Slesser and S. R. Schram (New York , Toronto, London: McGraw-Hill Book Company, Inc., 1951) at p. 817) in 300 ml ethanol was hydrogenated in a stainless steel autoclave with hydrogen for 3 hours at 20° C. and for 1 hour at 100° C. in the presence of potassium hydroxide (12 g) and Raney nickel (25 g). The pressure was in the range from 30 to 40 bar. The solid constituents were separated from the reaction mixture by filtration and the filtrate was distilled to give 16 g of 1,1,1,4,4,4-hexafluorobutane, boiling point 25°-30° C. at 1013 mbar. The mass spectrum showed an m+ /e of 166. The solid constituents were separated from the reaction mixture by filtration the filtrate was distilled

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

実験手順: In a 20 1 stainless steel autoclave, which had previously been conditioned using 10% strength nitric acid and was equipped with closed circuit heating and an anchor stirrer, 10.0 kg of 1,1,1,4,4,4-hexafluorobutene were heated from 0 to 30 C. over a period of 10 minutes in the presence of 250 g of catalyst (5% by weight of metallic palladium on activated carbon) at a pressure of 20 bar of hydrogen. After reaching this temperature, the hydrogen consumption was compensated for by repeated pressurization with fresh hydrogen at pressures between 20 and 30 bar. After about 2.5 hours the conversion was 87%. 1,1,1,4,4,4-Hexafluorobutane had been formed in a yield of greater than 99% of theory. was equipped with closed circuit heating the hydrogen consumption