2,2,3,3,4,4,5,5,5-nonafluoropentanoyl fluoride

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture consisting of 775 g of perfluoropentanoyl fluoride, 800 g of anhydrous diglyme, 13.1 g of potassium fluoride, 17.8 g of anhydrous potassium bifluoride and 775 g of hexafluoropropylene was heated in a 3-liter stainless steel pressure vessel under autogeneous pressure at 50° C. for 16 hours. The product was fractionally distilled to give 413 g of 1,1,1,2,4,4,5,5,6,6,7,7,7-tridecafluoro-2-trifluoromethyl-heptan-3-one, having a boiling point of 97° C. and a 99.0% purity as determined by gas chromatography and mass spectroscopy. The product was fractionally distilled

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture consisting of 775 g of perfluoropentanoyl fluoride, 800 g of anhydrous diglyme, 13.1 g of potassium fluoride, 17.8 g of anhydrous potassium bifluoride and 775 g of hexafluoropropylene was heated in a 3-liter stainless steel pressure vessel under autogeneous pressure at 50° C. for 16 hours. The product was fractionally distilled to give 413 g of 1,1,1,2,4,4,5,5,6,6,7,7,7-tridecafluoro-2-trifluoromethyl-heptan-3-one, having a boiling point of 97° C. and a 99.0% purity as determined by gas chromatography and mass spectroscopy. The product was fractionally distilled

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture consisting of 775 g of perfluoropentanoyl fluoride, 800 g of anhydrous diglyme, 13.1 g of potassium fluoride, 17.8 g of anhydrous potassium bifluoride and 775 g of hexafluoropropylene was heated in a 3-liter stainless steel pressure vessel under autogeneous pressure at 50° C. for 16 hours. The product was fractionally distilled to give 413 g of 1,1,1,2,4,4,5,5,6,6,7,7,7-tridecafluoro-2-trifluoromethyl-heptan-3-one, having a boiling point of 97° C. and a 99.0% purity as determined by gas chromatography and mass spectroscopy. The product was fractionally distilled

反応条件: temp:85.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A clean, dry, 600 mL, stainless steel, Parr pressure reactor was charged with spray-dried potassium fluoride (8.4 grams, 0.14 mole), anhydrous diglyme (128 grams), and Adogen™ 464 phase transfer catalyst (2.2 grams). The reactor was sealed, cooled with a dry ice-acetone bath, evacuated, and charged with perfluorovaleryl fluoride (130.0 grams, 0.49 mole) and C3F7OCF═CF2 (125.0 grams, 0.47 mole). The reactor was then heated to 85° C. and held for 20 hours with agitation. The reactor was cooled to below 0° C. with a dry ice-acetone bath and vented. The reactor contents were added to a clean, dry 2 L round bottom flask equipped with a mechanical stirrer, a heating mantle, a temperature probe, and a water condenser. The flask was charged with spray-dried potassium fluoride (16.0 grams, 0.28 mole), diethyl sulfate (61.0 grams, 0.40 mole), anhydrous diglyme (48 grams), and catalyst (2.5 grams). The contents of the flask were stirred, heated to 52° C., and held for 20 hours. The flask was cooled to ambient temperature, and water (35 grams) and 45 percent KOH (75 grams, 0.60 mole) were added. The flask was heated to 65° C. and held for 4 hours to neutralize excess diethyl sulfate. The resulting crude product was isolated by steam distillation, washed one time with an equal weight of water, and fractionally distilled to provide 91.0 grams of 99.3 percent purity product C3F7OCF(CF3)CF(OC2H5)C4F9. The boiling point of this product was 178° C., and its structure was confirmed by GCMS. The viscosity of the product was 7.3×10−5 m2/s (73 centistokes) at −50° C. (measured using a Cannon-Fenske viscometer and a Wescan Model 221 viscosity timer). A clean, dry The reactor was sealed cooled with a dry ice-acetone bath evacuated The reactor was cooled to below 0° C. with a dry ice-acetone bath The reactor contents were added to a clean, dry 2 L round bottom flask equipped with a mechanical stirrer heated to 52° C. held for 20 hours The flask was cooled to ambient temperature The flask was heated to 65° C. held for 4 hours The resulting crude product was isolated by steam distillation washed one time with an equal weight of water fractionally distilled

反応条件: temp:85.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A clean, dry, 600 mL, stainless steel, Parr pressure reactor was charged with spray-dried potassium fluoride (8.4 grams, 0.14 mole), anhydrous diglyme (128 grams), and Adogen™ 464 phase transfer catalyst (2.2 grams). The reactor was sealed, cooled with a dry ice-acetone bath, evacuated, and charged with perfluorovaleryl fluoride (130.0 grams, 0.49 mole) and C3F7OCF═CF2 (125.0 grams, 0.47 mole). The reactor was then heated to 85° C. and held for 20 hours with agitation. The reactor was cooled to below 0° C. with a dry ice-acetone bath and vented. The reactor contents were added to a clean, dry 2 L round bottom flask equipped with a mechanical stirrer, a heating mantle, a temperature probe, and a water condenser. The flask was charged with spray-dried potassium fluoride (16.0 grams, 0.28 mole), diethyl sulfate (61.0 grams, 0.40 mole), anhydrous diglyme (48 grams), and catalyst (2.5 grams). The contents of the flask were stirred, heated to 52° C., and held for 20 hours. The flask was cooled to ambient temperature, and water (35 grams) and 45 percent KOH (75 grams, 0.60 mole) were added. The flask was heated to 65° C. and held for 4 hours to neutralize excess diethyl sulfate. The resulting crude product was isolated by steam distillation, washed one time with an equal weight of water, and fractionally distilled to provide 91.0 grams of 99.3 percent purity product C3F7OCF(CF3)CF(OC2H5)C4F9. The boiling point of this product was 178° C., and its structure was confirmed by GCMS. The viscosity of the product was 7.3×10−5 m2/s (73 centistokes) at −50° C. (measured using a Cannon-Fenske viscometer and a Wescan Model 221 viscosity timer). A clean, dry The reactor was sealed cooled with a dry ice-acetone bath evacuated The reactor was cooled to below 0° C. with a dry ice-acetone bath The reactor contents were added to a clean, dry 2 L round bottom flask equipped with a mechanical stirrer heated to 52° C. held for 20 hours The flask was cooled to ambient temperature The flask was heated to 65° C. held for 4 hours The resulting crude product was isolated by steam distillation washed one time with an equal weight of water fractionally distilled

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture consisting of 775 g of perfluoropentanoyl fluoride, 800 g of anhydrous diglyme, 13.1 g of potassium fluoride, 17.8 g of anhydrous potassium bifluoride and 775 g of hexafluoropropylene was heated in a 3-liter stainless steel pressure vessel under autogeneous pressure at 50° C. for 16 hours. The product was fractionally distilled to give 413 g of 1,1,1,2,4,4,5,5,6,6,7,7,7-tridecafluoro-2-trifluoromethyl-heptan-3-one, having a boiling point of 97° C. and a 99.0% purity as determined by gas chromatography and mass spectroscopy. The product was fractionally distilled

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture consisting of 775 g of perfluoropentanoyl fluoride, 800 g of anhydrous diglyme, 13.1 g of potassium fluoride, 17.8 g of anhydrous potassium bifluoride and 775 g of hexafluoropropylene was heated in a 3-liter stainless steel pressure vessel under autogeneous pressure at 50° C. for 16 hours. The product was fractionally distilled to give 413 g of 1,1,1,2,4,4,5,5,6,6,7,7,7-tridecafluoro-2-trifluoromethyl-heptan-3-one, having a boiling point of 97° C. and a 99.0% purity as determined by gas chromatography and mass spectroscopy. The product was fractionally distilled

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture consisting of 775 g of perfluoropentanoyl fluoride, 800 g of anhydrous diglyme, 13.1 g of potassium fluoride, 17.8 g of anhydrous potassium bifluoride and 775 g of hexafluoropropylene was heated in a 3-liter stainless steel pressure vessel under autogeneous pressure at 50° C. for 16 hours. The product was fractionally distilled to give 413 g of 1,1,1,2,4,4,5,5,6,6,7,7,7-tridecafluoro-2-trifluoromethyl-heptan-3-one, having a boiling point of 97° C. and a 99.0% purity as determined by gas chromatography and mass spectroscopy. The product was fractionally distilled

反応条件: temp:85.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A clean, dry, 600 mL, stainless steel, Parr pressure reactor was charged with spray-dried potassium fluoride (8.4 grams, 0.14 mole), anhydrous diglyme (128 grams), and Adogen™ 464 phase transfer catalyst (2.2 grams). The reactor was sealed, cooled with a dry ice-acetone bath, evacuated, and charged with perfluorovaleryl fluoride (130.0 grams, 0.49 mole) and C3F7OCF═CF2 (125.0 grams, 0.47 mole). The reactor was then heated to 85° C. and held for 20 hours with agitation. The reactor was cooled to below 0° C. with a dry ice-acetone bath and vented. The reactor contents were added to a clean, dry 2 L round bottom flask equipped with a mechanical stirrer, a heating mantle, a temperature probe, and a water condenser. The flask was charged with spray-dried potassium fluoride (16.0 grams, 0.28 mole), diethyl sulfate (61.0 grams, 0.40 mole), anhydrous diglyme (48 grams), and catalyst (2.5 grams). The contents of the flask were stirred, heated to 52° C., and held for 20 hours. The flask was cooled to ambient temperature, and water (35 grams) and 45 percent KOH (75 grams, 0.60 mole) were added. The flask was heated to 65° C. and held for 4 hours to neutralize excess diethyl sulfate. The resulting crude product was isolated by steam distillation, washed one time with an equal weight of water, and fractionally distilled to provide 91.0 grams of 99.3 percent purity product C3F7OCF(CF3)CF(OC2H5)C4F9. The boiling point of this product was 178° C., and its structure was confirmed by GCMS. The viscosity of the product was 7.3×10−5 m2/s (73 centistokes) at −50° C. (measured using a Cannon-Fenske viscometer and a Wescan Model 221 viscosity timer). A clean, dry The reactor was sealed cooled with a dry ice-acetone bath evacuated The reactor was cooled to below 0° C. with a dry ice-acetone bath The reactor contents were added to a clean, dry 2 L round bottom flask equipped with a mechanical stirrer heated to 52° C. held for 20 hours The flask was cooled to ambient temperature The flask was heated to 65° C. held for 4 hours The resulting crude product was isolated by steam distillation washed one time with an equal weight of water fractionally distilled