2,2,3,3,3-pentafluoropropanoyl fluoride

反応条件: temp:-20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A jacketed one liter round bottom flask was equipped with an overhead stirrer, a solid carbon dioxide/acetone condenser, and an addition funnel. The flask was charged with spray-dried potassium fluoride (85 g, 1.46 mol) and anhydrous diethylene glycol dimethyl ether (375 g) and was then cooled to about −20° C. using a recirculating refrigeration system. C2F5COF (196 g, 1.18 mol) was added to the flask over a period of about one hour. The flask was then warmed to about 24° C., and dimethyl sulfate (184.3 g, 1.46 mol) was then added dropwise via the addition funnel over a 45 minute period. The resulting mixture was then stirred at room temperature overnight. Water (a total of 318 mL) was then added dropwise to the mixture. The mixture was transferred to a one liter round bottom flask, and the resulting product ether was azeotropically distilled. The lower product phase of the resulting distillate was separated from the upper aqueous phase, was washed once with cold water, and was subsequently distilled to give 180 g of product (b.p. 36° C.;>99.9% purity by GLC). The product identity was confirmed by GCMS and by 1H and 19F NMR. A jacketed one liter round bottom flask was equipped with an overhead stirrer, a solid carbon dioxide/acetone condenser, and an addition funnel The flask was then warmed to about 24° C. The mixture was transferred to a one liter round bottom flask the resulting product ether was azeotropically distilled The lower product phase of the resulting distillate was separated from the upper aqueous phase was washed once with cold water was subsequently distilled

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

実験手順: CF3CF2COF (b.p. -28° C.) is prepared by flowing hexafluoropropylene oxide through a stainless steel reactor tube containing active carbon carrying 3% by weight of potassium fluoride kept at 150° C. kept at 150° C.

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

実験手順: CF3CF2COF (b.p. -28° C.) is prepared by flowing hexafluoropropylene oxide through a stainless steel reactor tube containing active carbon carrying 3% by weight of potassium fluoride kept at 150° C. kept at 150° C.

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

実験手順: HO(CH2)2O(CH2)2OCH(CH3)CH2OH (5.1 g) obtained in Example 5-2 and chloroform (10 g) were charged into a flask and stirred while maintaining the internal temperature at 30° C. Together with nitrogen, CF3CF2COF (191 g) was supplied while maintaining the internal temperature at 30° C. After completion of the reaction, while supplying nitrogen gas, stirring was continued at an internal temperature of 30° C. for 2 hours, and then, a 5% NaHCO3 aqueous solution (30 ml) was added at an internal temperature of at most 15° C. while maintaining the internal temperature at 30° C After completion of the reaction stirring

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

実験手順: HO(CH2)2O(CH2)2OCH(CH3)CH2OH (5.1 g) obtained in Example 5-2 and chloroform (10 g) were charged into a flask and stirred while maintaining the internal temperature at 30° C. Together with nitrogen, CF3CF2COF (191 g) was supplied while maintaining the internal temperature at 30° C. After completion of the reaction, while supplying nitrogen gas, stirring was continued at an internal temperature of 30° C. for 2 hours, and then, a 5% NaHCO3 aqueous solution (30 ml) was added at an internal temperature of at most 15° C. while maintaining the internal temperature at 30° C After completion of the reaction stirring

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

実験手順: HO(CH2)2O(CH2)2OH (40 g) was put into a flask and stirred while maintaining the internal temperature at 30° C. While maintaining the internal temperature of the flask at 30° C., nitrogen and CF3CF2COF (388 g) were supplied over a period of 1.5 hours. After completion of the reaction, while supplying nitrogen gas, stirring was continued at an internal temperature of 30° C. for 2 hours, and then the internal temperature of the flask was brought to at most 15° C., whereupon 5% NaHCO3 (300 ml) was added. While maintaining the internal temperature of the flask at 30° C. After completion of the reaction stirring was added

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

実験手順: HO(CH2)2O(CH2)2OH (40 g) was put into a flask and stirred while maintaining the internal temperature at 30° C. While maintaining the internal temperature of the flask at 30° C., nitrogen and CF3CF2COF (388 g) were supplied over a period of 1.5 hours. After completion of the reaction, while supplying nitrogen gas, stirring was continued at an internal temperature of 30° C. for 2 hours, and then the internal temperature of the flask was brought to at most 15° C., whereupon 5% NaHCO3 (300 ml) was added. While maintaining the internal temperature of the flask at 30° C. After completion of the reaction stirring was added

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

実験手順: HO(CH2)4OCH(CH3)CH2OH (18.8 g) obtained in Example 2-3 was put into a round bottom flask and stirred while maintaining the internal temperature at 30° C. Together with nitrogen, CF3CF2COF (276 g) was supplied over 6 hours while maintaining the internal temperature at 30° C. After completion of the reaction, stirring was continued for 2 hours at an internal temperature of 30° C. while supplying nitrogen gas, whereupon a 5% NaHCO3 aqueous solution (300 ml) was added at an internal temperature of at most 15° C. while maintaining the internal temperature at 30° C After completion of the reaction stirring

反応条件: temp:200.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: CF3CF2COOCF2CF2CF3 (20 g) obtained in Example 5 and chlorotrifluoroethylene oligomer (120 g) were charged into a 200 ml autoclave made of nickel and equipped with a reflux condenser and heated to 200° C. The reflux condenser was cooled by circulating cooling water, and when the pressure became at least 0.1 MPa, the gas was purged while maintaining the pressure to recover a gaseous sample (15 g). By GC-MS, it was confirmed that CF3CF2COF was the main product. The GC yield was 90%. equipped with a reflux condenser The reflux condenser was cooled the gas was purged while maintaining the pressure to recover a gaseous sample (15 g)

反応条件: temp:200.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: CF3CF2COOCF2CF2CF3 (20 g) obtained in Example 5 and chlorotrifluoroethylene oligomer (120 g) were charged into a 200 ml autoclave made of nickel and equipped with a reflux condenser and heated to 200° C. The reflux condenser was cooled by circulating cooling water, and when the pressure became at least 0.1 MPa, the gas was purged while maintaining the pressure to recover a gaseous sample (15 g). By GC-MS, it was confirmed that CF3CF2COF was the main product. The GC yield was 90%. equipped with a reflux condenser The reflux condenser was cooled the gas was purged while maintaining the pressure to recover a gaseous sample (15 g)

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

実験手順: CH3COCH2OH (150.0 g) and triethylamine (225.4 g) were put into a flask and stirred under cooling in an ice bath. CF3CF2COF (377.5 g) diluted with nitrogen gas was blown into the flask over a period of 4 hours, while maintaining the internal temperature to be at most 10° C. Then, the mixture was stirred at room temperature for 2 hours and then added to 500 mL of ice water. under cooling in an ice bath while maintaining the internal temperature to be at most 10° C Then, the mixture was stirred at room temperature for 2 hours

反応条件: temp:-20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A jacketed one liter round bottom flask was equipped with an overhead stirrer, a solid carbon dioxide/acetone condenser, and an addition funnel. The flask was charged with spray-dried potassium fluoride (85 g, 1.46 mol) and anhydrous diethylene glycol dimethyl ether (375 g) and was then cooled to about -20° C. using a recirculating refrigeration system. C2F5COF (196 g, 1.18 mol) was added to the flask over a period of about one hour. The flask was then warmed to about 24° C., and dimethyl sulfate (184.3 g, 1.46 mol) was then added dropwise via the addition funnel over a 45 minute period. The resulting mixture was then stirred at room temperature overnight. Water (a total of 318 mL) was then added dropwise to the mixture. The mixture was transferred to a one liter round bottom flask, and the resulting product ether was azeotropically distilled. The lower product phase of the resulting distillate was separated from the upper aqueous phase, was washed once with cold water, and was subsequently distilled to give 180 g of product (b.p. 36° C.; >99.9% purity by GLC). The product identity was confirmed by GCMS and by 1H and 19F NMR. A jacketed one liter round bottom flask was equipped with an overhead stirrer, a solid carbon dioxide/acetone condenser, and an addition funnel The flask was then warmed to about 24° C. The mixture was transferred to a one liter round bottom flask the resulting product ether was azeotropically distilled The lower product phase of the resulting distillate was separated from the upper aqueous phase was washed once with cold water was subsequently distilled