1,1,3-trichloro-1,2,2,3,3-pentafluoropropane

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

実験手順: 106.6 grams (0.45 mol) 1,1,3-trichloro-1,2,2,3,3-pentafluoropropane (produced in Part C above) and 300 gm (5 mol) isopropanol were stirred under an inert atmosphere and irradiated 4.5 hours with a 450 W Hanovia Hg lamp at a distance of 2-3 inches (5-7.6 cm). The acidic reaction mixture was then poured into 1.5 liters ice water. The organic layer was separated, washed twice with 50 ml water, dried with calcium sulfate, and distilled to give 50.5 gm ClCF2CF2CHClF, bp 54.5-56° C. (55%). 1H NMR (CDCl3): ddd centered at 6.43 ppm. J H-C-F=47 Hz, J H-C-C-Fa=12 Hz, J H-C-C-Fb=2 Hz. irradiated 4.5 hours with a 450 W Hanovia Hg lamp at a distance of 2-3 inches (5-7.6 cm) The organic layer was separated washed twice with 50 ml water dried with calcium sulfate distilled

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

実験手順: 1,1,3-trichloro-1,2,2,3,3-pentafluoropropane(produced in Part C above) (106.6 g, 0.45 mol) and 300 g(5 mol) isopropanol were stirred under an inert atmosphere and irradiated 4.5 hours with a 450 W Hanovia Hg lamp at a distance of 2-3 inches(5-7.6 cm). The acidic reaction mixture was then poured into 1.5 liters ice water. The organic layer was separated, washed twice with 50 ml water, dried with calcium sulfate, and distilled to give 50.5 g ClCF2CF2CHClF, bp 54.5°-56° C. (55%). 1H NMR (CDCl3): ddd centered at 6.43 ppm. J H--C--F=47 Hz, J H--C--C--Fa=12 Hz, J H--C--C--Fb=2 Hz. irradiated 4.5 hours with a 450 W Hanovia Hg lamp at a distance of 2-3 inches(5-7.6 cm) The organic layer was separated washed twice with 50 ml water dried with calcium sulfate distilled

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

実験手順: For example, to prepare 1,3-dichloro-1,1,2,2,3-pentafluoropropane, 2,2,3,3-tetrafluoropropanol, tosyl chloride, and water are reacted together to form 2,2,3,3-tetrafluoropropyl p-toluenesulfonate. Then, N-methylpyrrolidone, potassium fluoride, and the 2,2,3,3-tetrafluoropropyl p-toluenesulfonate are reacted together to form 1,1,2,2,3-pentafluoropropane. Then, chlorine and the 1,1,2,2,3-pentafluoropropane are reacted to form 1,1,3-trichloro-1,2,2,3,3-pentafluoropropane. Finally, isopropanol and the 1,1,3-trichloro-1,2,2,3,3-pentafluoropropane are reacted to form 1,3-dichloro-1,1,2,2,3-pentafluoropropane.

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

実験手順: 106.6 grams (0.45 mol) 1,1,3-trichloro-1,2,2,3,3-pentafluoropropane (produced in Part C above) and 300 gm (5 mol) isopropanol were stirred under an inert atmosphere and irradiated 4.5 hours with a 450 W Hanovia Hg lamp at a distance of 2-3 inches (5-7.6 cm). The acidic reaction mixture was then poured into 1.5 liters ice water. The organic layer was separated, washed twice with 50 ml water, dried with calcium sulfate, and distilled to give 50.5 gm ClCF2CF2CHClF, bp 54.5-56° C. (55%). 1H NMR (CDCl3): ddd centered at 6.43 ppm. J H-C-F=47 Hz, J H-C-C-Fa=12 Hz, J H-C-C-Fb=2 Hz. irradiated 4.5 hours with a 450 W Hanovia Hg lamp at a distance of 2-3 inches (5-7.6 cm) The organic layer was separated washed twice with 50 ml water dried with calcium sulfate distilled