3,3,3-trifluoro-2-(trifluoromethyl)prop-1-ene

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: In the form of the present invention starting from hexafluoropropylene oxide, a vapor stream of hexafluoropropylene oxide is fed at any convenient flow rate, e.g., in the range of about 0.04 to about 0.06 g-mole/hr to a reactor maintained at a temperature in the range of about 400° to about 650° C. and containing a fluorinated catalyst (hereinafter described) for a residence time sufficient to for a vapor stream comprising hexafluoroacetone which is not isolated but forwarded directly to a heating zone of the reactor for conversion to hexafluoroisobutylene. maintained at a temperature in the range of about 400° to about 650° C. containing a fluorinated catalyst (

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

実験手順: In the form of the present invention starting from hexafluoropropylene oxide, a vapor stream of hexafluoropropylene oxide is fed at any convenient flow rate, e.g., in the range of about 0.04 to about 0.06 g-mole/hr to a reactor maintained at a temperature in the range of about 400° to about 650° C. and containing a fluorinated catalyst (hereinafter described) for a residence time sufficient to for a vapor stream comprising hexafluoroacetone which is not isolated but forwarded directly to a heating zone of the reactor for conversion to hexafluoroisobutylene. maintained at a temperature in the range of about 400° to about 650° C. containing a fluorinated catalyst (

反応条件: temp:65.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a four necked 100 ml flask equipped with a condenser, a dropping funnel and a thermometer, tributylamine (20.0 g, 108 mmoles) was charged and warmed to 65° C. Monochloromethyl 2-trifluoromethyl-3,3,3-trifluoropropanoate (4.88 g, 20 mmol) was dropwise added thereto while stirring. The reaction was continued at the same temperature as above for 3 hours while stirring. The gas evolved from a top of the condenser was washed with an alkaline solution, dried with alumina and cooled. The resultant liquid was distilled to give 2-trifluoromethyl-3,3,3-trifluoropropene (2.49 g). Yield, 76 %. In a four necked 100 ml flask equipped with a condenser, a dropping funnel was continued at the same temperature as above for 3 hours while stirring was washed with an alkaline solution dried with alumina cooled The resultant liquid was distilled

反応条件: temp:65.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a four necked 100 ml flask equipped with a condenser, a dropping funnel and a thermometer, tributylamine (20.0 g, 108 mmoles) was charged and warmed to 65° C. Monochloromethyl 2-trifluoromethyl-3,3,3-trifluoropropanoate (4.88 g, 20 mmol) was dropwise added thereto while stirring. The reaction was continued at the same temperature as above for 3 hours while stirring. The gas evolved from a top of the condenser was washed with an alkaline solution, dried with alumina and cooled. The resultant liquid was distilled to give 2-trifluoromethyl-3,3,3-trifluoropropene (2.49 g). Yield, 76 %. In a four necked 100 ml flask equipped with a condenser, a dropping funnel was continued at the same temperature as above for 3 hours while stirring was washed with an alkaline solution dried with alumina cooled The resultant liquid was distilled

反応条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a four necked 100 ml flask equipped with a condenser, a dropping funnel and a thermometer, triethylamine (20.0 g, 198 mmol) was charged and warmed to 60° C. Monochloromethyl 2-trifluoromethyl-3,3,3-trifluoropropanoate (4.88 g, 20 mmol) was dropwise added thereto while stirring. The reaction was continued at the same temperature as above for 2.5 hours while stirring. The gas evolved from a top of the condenser was washed with an alkaline solution, dried with alumina and cooled. The resultant liquid was distilled to give 2-trifluoromethyl-3,3,3-trifluoropropene (2.36 g). Yield, 72 %. In a four necked 100 ml flask equipped with a condenser, a dropping funnel was continued at the same temperature as above for 2.5 hours while stirring was washed with an alkaline solution dried with alumina cooled The resultant liquid was distilled

反応条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a four necked 100 ml flask equipped with a condenser, a dropping funnel and a thermometer, pyridine (19.3 g, 244 mmol) was charged and warmed to 70° C. Monochloromethyl 2-trifluoromethyl-3,3,3-trifluoropropanoate (4.88 g, 20 mmol) was dropwise added thereto while stirring. The reaction was continued at the same temperature as above for 2 hours while stirring. The gas evolved from a top of the condenser was washed with an alkaline solution, dried with alumina and cooled. The resultant liquid was distillated to give 2-trifluoromethyl-3,3,3-trifluoropropene (b.p., 14° C.) (2.30 g). Yield, 70 %. In a four necked 100 ml flask equipped with a condenser, a dropping funnel was continued at the same temperature as above for 2 hours while stirring was washed with an alkaline solution dried with alumina cooled

反応条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a four necked 100 ml flask equipped with a condenser, a dropping funnel and a thermometer, pyridine (19.3 g, 244 mmol) was charged and warmed to 70° C. Monochloromethyl 2-trifluoromethyl-3,3,3-trifluoropropanoate (4.88 g, 20 mmol) was dropwise added thereto while stirring. The reaction was continued at the same temperature as above for 2 hours while stirring. The gas evolved from a top of the condenser was washed with an alkaline solution, dried with alumina and cooled. The resultant liquid was distillated to give 2-trifluoromethyl-3,3,3-trifluoropropene (b.p., 14° C.) (2.30 g). Yield, 70 %. In a four necked 100 ml flask equipped with a condenser, a dropping funnel was continued at the same temperature as above for 2 hours while stirring was washed with an alkaline solution dried with alumina cooled

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

実験手順: Among the thus produced fluorine-containing compounds (I), monochloromethyl 2-trifluoromethyl-3,3,3-trifluoropropanoate is reacted with an amine to give 2-trifluoromethyl-3,3,3-trifluoropropene in a high yield.

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

実験手順: Among the thus produced fluorine-containing compounds (I), monochloromethyl 2-trifluoromethyl-3,3,3-trifluoropropanoate is reacted with an amine to give 2-trifluoromethyl-3,3,3-trifluoropropene in a high yield.

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

実験手順: 5.2 g (20 mmol) of the Diels-Alder reaction product of 3,3,3-trifluoro-2-trifluoromethyl-1-propene (hexafluoroisobutene) and cyclopentadiene are mixed with 20 ml of formic acid, and 1.3 ml of 70 percent strength hydrogen peroxide (30 mmol) is added at 50° C., and the mixture is held at 50° C. for 20 hours. Testing for oxidant using KI-starch paper showed that the oxidant had been broken down completely. The low-boiling components are distilled off under reduced pressure. The residue is heated to 50° C. with 200 ml of 20% strength aqueous sodium hydroxide. The precipitated solid is extracted with a total of 130 ml of methylene chloride. The combined extracts are dried with magnesium sulfate, the methylene chloride is distilled off, and the residue is sublimated at 60° C. in an oil pump vacuum. is added at 50° C. The low-boiling components are distilled off under reduced pressure The precipitated solid is extracted with a total of 130 ml of methylene chloride The combined extracts are dried with magnesium sulfate the methylene chloride is distilled off is sublimated at 60° C. in an oil pump vacuum

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

実験手順: 5.2 g (20 mmol) of the Diels-Alder reaction product of 3,3,3-trifluoro-2-trifluoromethyl-1-propene (hexafluoroisobutene) and cyclopentadiene are mixed with 20 ml of formic acid, and 1.3 ml of 70 percent strength hydrogen peroxide (30 mmol) is added at 50° C., and the mixture is held at 50° C. for 20 hours. Testing for oxidant using KI-starch paper showed that the oxidant had been broken down completely. The low-boiling components are distilled off under reduced pressure. The residue is heated to 50° C. with 200 ml of 20% strength aqueous sodium hydroxide. The precipitated solid is extracted with a total of 130 ml of methylene chloride. The combined extracts are dried with magnesium sulfate, the methylene chloride is distilled off, and the residue is sublimated at 60° C. in an oil pump vacuum. is added at 50° C. The low-boiling components are distilled off under reduced pressure The precipitated solid is extracted with a total of 130 ml of methylene chloride The combined extracts are dried with magnesium sulfate the methylene chloride is distilled off is sublimated at 60° C. in an oil pump vacuum