三氟乙酰氟

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: The procedure described in Example 9 is employed in which 10.2 grams hexafluoropropylene is condensed in at high pressure and 12 grams liquid carbon dioxide is added. The temperature is raised to 60° C., and the cell is charged with molecular oxygen to approximately 2,500 psi. Oxygen is supplied continuously to the reactor. 0.5 grams of a clear fluid is collected in the cold trap corresponding to a 5% yield of perfluoropolyether (based on hexafluoropropylene). Analysis using 19F NMR spectroscopy is consistent with a perfluoropolyether structure. Analysis of portions of the gaseous products shows evidence of carbonyl fluoride and trifluoroacetyl fluoride in addition to other low molar mass fluorooxy compounds.

反应条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Trifluoroacetyl fluoride (6 g, 0.051 mole) is bubbled into a mixture of KF (2.4 g, 0.041 mole) and dry diglyme (15 ml). The reaction mixture is stirred at 20° C. for 30 minutes and then CH2═C(CF3)CF2OSO2F (10 g, 0.041 mile) is added gradually. The resulting mixture is stirred at 20° C. for 1 hour. Hexafluoroisobutylene is distilled from the reaction mixture and the residue is poured into water. The organic layer. is separated, washed in turn with aqueous sodium bicarbonate solution and water, and then dried over MgSO4. Distillation gives 3,3-Difluoro-3-pentafluoroethoxy-2-trifluoromethylpropene (CH2═C(CF3)CF2OCF2CF3) (3.5 g, 31% yield, b.pt. 67° C.). The resulting mixture is stirred at 20° C. for 1 hour Hexafluoroisobutylene is distilled from the reaction mixture the residue is poured into water is separated washed in turn with aqueous sodium bicarbonate solution and water dried over MgSO4 Distillation

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: The procedure described in Example 9 is employed in which 10.2 grams hexafluoropropylene is condensed in at high pressure and 12 grams liquid carbon dioxide is added. The temperature is raised to 60° C., and the cell is charged with molecular oxygen to approximately 2,500 psi. Oxygen is supplied continuously to the reactor. 0.5 grams of a clear fluid is collected in the cold trap corresponding to a 5% yield of perfluoropolyether (based on hexafluoropropylene). Analysis using 19F NMR spectroscopy is consistent with a perfluoropolyether structure. Analysis of portions of the gaseous products shows evidence of carbonyl fluoride and trifluoroacetyl fluoride in addition to other low molar mass fluorooxy compounds.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: The procedure described in Example 9 is employed in which 10.2 grams hexafluoropropylene is condensed in at high pressure and 12 grams liquid carbon dioxide is added. The temperature is raised to 60° C., and the cell is charged with molecular oxygen to approximately 2,500 psi. Oxygen is supplied continuously to the reactor. 0.5 grams of a clear fluid is collected in the cold trap corresponding to a 5% yield of perfluoropolyether (based on hexafluoropropylene). Analysis using 19F NMR spectroscopy is consistent with a perfluoropolyether structure. Analysis of portions of the gaseous products shows evidence of carbonyl fluoride and trifluoroacetyl fluoride in addition to other low molar mass fluorooxy compounds.

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Trifluoroacetyl fluoride (6 g, 0.051 mole) is bubbled into a mixture of KF (2.4 g, 0.041 mole) and dry diglyme (15 ml). The reaction mixture is stirred at 20° C. for 30 minutes and then CH2═C(CF3)CF2OSO2F (10 g, 0.041 mile) is added gradually. The resulting mixture is stirred at 20° C. for 1 hour. Hexafluoroisobutylene is distilled from the reaction mixture and the residue is poured into water. The organic layer. is separated, washed in turn with aqueous sodium bicarbonate solution and water, and then dried over MgSO4. Distillation gives 3,3-Difluoro-3-pentafluoroethoxy-2-trifluoromethylpropene (CH2═C(CF3)CF2OCF2CF3) (3.5 g, 31% yield, b.pt. 67° C.). The resulting mixture is stirred at 20° C. for 1 hour Hexafluoroisobutylene is distilled from the reaction mixture the residue is poured into water is separated washed in turn with aqueous sodium bicarbonate solution and water dried over MgSO4 Distillation

反应条件: temp:-30.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: At −30° C., trifluoroacetyl fluoride (18.3 g, 0.16 mol; 99.5%) was introduced into a solution of methyl 3-piperidin-1-ylacrylate (97%, 25 g, 0.14 mol) and KF (12.5 g, 0.51 mol) in toluene (250 ml). The reaction mixture was stirred at −30° C. for 3 h and then, over a period of one hour, warmed to room temperature. The reaction mixture was washed with deionized water (400 ml). After phase separation, the aqueous phase was extracted once with toluene (200 ml). The toluene phases were combined and, under reduced pressure, concentrated to about 600 ml. The reaction solution obtained in this manner was, at −50° C., added dropwise to a solution of methylhydrazine (7.4 g, 0.16 mol) in toluene (150 ml). The reaction mixture was stirred at −50° C. for 2 h and then, over a period of one hour, warmed to room temperature. Aqueous sodium hydroxide solution (10% strength, 69.4 g, 0.17 mol) was then added, and the reaction mixture was heated under reflux conditions for 2 h. After cooling to room temperature, the phases were separated. The toluene phase was extracted with aqueous sodium hydroxide solution (10% strength, 100 ml). The aqueous phases were combined, adjusted to pH 1 using hydrochloric acid (conc.) and cooled to 0° C. The precipitated solid was filtered off, washed with cyclohexane and, at 60° C., dried under reduced pressure. 3-trifluoromethyl-1-methyl-1H-pyrazol-4-ylcarboxylic acid was obtained in an amount of 21.8 g and a purity of 98% (according to 1H-NMR) (yield: 0.12 mol, 81%). over a period of one hour warmed to room temperature The reaction mixture was washed with deionized water (400 ml) After phase separation the aqueous phase was extracted once with toluene (200 ml) concentrated to about 600 ml The reaction solution obtained in this manner was, at −50° C. The reaction mixture was stirred at −50° C. for 2 h over a period of one hour warmed to room temperature the reaction mixture was heated under reflux conditions for 2 h After cooling to room temperature the phases were separated The toluene phase was extracted with aqueous sodium hydroxide solution (10% strength, 100 ml) cooled to 0° C The precipitated solid was filtered off washed with cyclohexane and, at 60° C. dried under reduced pressure

反应条件: temp:-30.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Methyl 3-piperidin-1-ylacrylate (97%, 25 g, 0.14 mol) and KF (12.5 g, 76.3 mmol) were initially charged in 250 ml of toluene and cooled to −30° C. At this temperature, trifluoroacetyl fluoride (99.5%, 18.3 g, 0.16 mol) was then introduced. The reaction mixture was stirred at −30° C. for 3 h and then, over a period of one hour, warmed to room temperature. The reaction mixture was washed with deionized water (100 ml). After phase separation, the aqueous phase was extracted once with toluene (100 ml). The toluene phases were combined, washed with an aqueous sat. NaCl solution (100 ml) and then freed from the solvent under reduced pressure. Methyl 4,4,4-trifluoro-3-oxo-2-(piperidin-1-ylmethylidene)butyrate was obtained as an orange solid (amount: 38.0 g; purity according to GC: 98%; yield: 98%). 1H-NMR (CDCl3): δ=1.75 (m, 6H), 3.3 (m, 2H), 3.6 (m, 2H), 3.75 (s, 3H), 7.65 ppm (s, 1H). over a period of one hour warmed to room temperature The reaction mixture was washed with deionized water (100 ml) After phase separation the aqueous phase was extracted once with toluene (100 ml) washed with an aqueous sat. NaCl solution (100 ml)

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: This exemplified compound may be readily synthesized by the reaction of methyl isocyanate with hydrazine to give 4-methyl-3-thiosemicarbazide followed by cyclocondensation with trifluoroacetic acid as described in U.S. Pat. No. 4,477,459. This compound may also be prepared by the reaction of 4-methyl-3-thiosemicarbazide with trifluoroacetylfluoride and heat (U.S. Pat. No. 3,780,052). heat (U.S

反应条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Trifluoroacetyl fluoride (6 g, 0.051 mole) is bubbled into a mixture of KF (2.4 g, 0.041 mole) and dry diglyme (15 ml). The reaction mixture is stirred at 20° C. for 30 minutes and then CH2═C(CF3)CF2OSO2F (10 g, 0.041 mile) is added gradually. The resulting mixture is stirred at 20° C. for 1 hour. Hexafluoroisobutylene is distilled from the reaction mixture and the residue is poured into water. The organic layer. is separated, washed in turn with aqueous sodium bicarbonate solution and water, and then dried over MgSO4. Distillation gives 3,3-Difluoro-3-pentafluoroethoxy-2-trifluoromethylpropene (CH2═C(CF3)CF2OCF2CF3) (3.5 g, 31% yield, b.pt. 67° C.). The resulting mixture is stirred at 20° C. for 1 hour Hexafluoroisobutylene is distilled from the reaction mixture the residue is poured into water is separated washed in turn with aqueous sodium bicarbonate solution and water dried over MgSO4 Distillation

反应条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Trifluoroacetyl fluoride (6 g, 0.051 mole) is bubbled into a mixture of KF (2.4 g, 0.041 mole) and dry diglyme (15 ml). The reaction mixture is stirred at 20° C. for 30 minutes and then CH2═C(CF3)CF2OSO2F (10 g, 0.041 mile) is added gradually. The resulting mixture is stirred at 20° C. for 1 hour. Hexafluoroisobutylene is distilled from the reaction mixture and the residue is poured into water. The organic layer is separated, washed in turn with aqueous sodium bicarbonate solution and water, and then dried over MgSO4. Distillation gives 3,3-Difluoro-3-pentafluoroethoxy-2-trifluoromethylpropene (CH2═C(CF3)CF2OCF2CF3) (3.5 g, 31% yield, b.pt. 67° C.). The resulting mixture is stirred at 20° C. for 1 hour Hexafluoroisobutylene is distilled from the reaction mixture the residue is poured into water The organic layer is separated washed in turn with aqueous sodium bicarbonate solution and water dried over MgSO4 Distillation