1,1,1,3,3,3-hexachloropropane

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

实验步骤: The known methods of producing 1,1,1,3,3-pentafluoropropane are as follows. Carbon tetrachloride and vinylidene chloride are prepared and an addition reaction is triggered. The reaction product, 1,1,1,3,3,3-hexachloropropane, is fluorinated to produce 1,1,1,3,3-pentafluoro-3-chloropropane which is reduced with hydrogen to produce 1,1,1,3,3-pentafluoropropane (WO 95/04022). an addition reaction

反应条件: temp:-10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 600 mL, magnetically stirred, model autoclave fitted with a condenser (maintained at -10° C.), was evacuated, cooled to about -40° C., and charged with 0.6.9 g (0.036 mol) TiCl4 followed by 64 g (0.255 mol) CCl3CH2CCl3, and 102.5 g (5 mol) HF. The temperature was increased to 120° C. and maintained at that temperature for a total of 22 h. During the heating period, pressure in excess of 400 psig was periodically vented to an aqueous KOH scrubber which was attached to two -78° C. cold traps. At the end of the heating period, the remainder of the autoclave contents were slowly vented. The cold traps contained 36.1 g material which by GC analysis, contained 14.5% CF3CH2CF3 and 84.0% CF3CH2 CF2Cl, corresponding to a yield for CF3CH2CF2Cl of 69%. model autoclave fitted with a condenser was evacuated cooled to about -40° C. The temperature was increased to 120° C. maintained at that temperature for a total of 22 h was attached to two -78° C.

反应条件: temp:-10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 600 mL, magnetically stirred, model autoclave fitted with a condenser (maintained at -10° C.), was evacuated, cooled to about -40° C., and charged with 0.6.9 g (0.036 mol) TiCl4 followed by 64 g (0.255 mol) CCl3CH2CCl3, and 102.5 g (5 mol) HF. The temperature was increased to 120° C. and maintained at that temperature for a total of 22 h. During the heating period, pressure in excess of 400 psig was periodically vented to an aqueous KOH scrubber which was attached to two -78° C. cold traps. At the end of the heating period, the remainder of the autoclave contents were slowly vented. The cold traps contained 36.1 g material which by GC analysis, contained 14.5% CF3CH2CF3 and 84.0% CF3CH2 CF2Cl, corresponding to a yield for CF3CH2CF2Cl of 69%. model autoclave fitted with a condenser was evacuated cooled to about -40° C. The temperature was increased to 120° C. maintained at that temperature for a total of 22 h was attached to two -78° C.

反应条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 400 mL Hastelloy™ C nickel alloy shaker tube was charged with anhydrous cuprous chloride (1.39 g, 0.014 mole), triethylamine hydrochloride (1.93 g, 0.014 mole), adiponitrile (52.0 g, 0.481 mole), carbon tetrachloride (151.0 g, 0.982 mole), and vinylidene chloride (47.5 g, 0.490 mole). The tube was sealed, cooled in a dry ice bath, evacuated, and purged with nitrogen several times. The tube was placed in a heating jacket and agitation begun. The tube was heated to 120° C. over the course of 1.3 hours and then held at 119-122° C. for one hour; during this time the pressure rose to a maximum of 83 psig (674 kPa) and then dropped to 41 psig (384 kPa) at the end of the heating period. The tube was then cooled to ambient temperature. The tube was sealed cooled in a dry ice bath evacuated purged with nitrogen several times dropped to 41 psig (384 kPa) at the end of the heating period The tube was then cooled to ambient temperature

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

实验步骤: The known methods of producing 1,1,1,3,3-pentafluoropropane are as follows. Carbon tetrachloride and vinylidene chloride are prepared and an addition reaction is triggered. The reaction product, 1,1,1,3,3,3-hexachloropropane, is fluorinated to produce 1,1,1,3,3-pentafluoro-3-chloropropane which is reduced with hydrogen to produce 1,1,1,3,3-pentafluoropropane (WO 95/04022). an addition reaction

反应条件: temp:-10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 600 mL, magnetically stirred, model autoclave fitted with a condenser (maintained at -10° C.), was evacuated, cooled to about -40° C., and charged with 0.6.9 g (0.036 mol) TiCl4 followed by 64 g (0.255 mol) CCl3CH2CCl3, and 102.5 g (5 mol) HF. The temperature was increased to 120° C. and maintained at that temperature for a total of 22 h. During the heating period, pressure in excess of 400 psig was periodically vented to an aqueous KOH scrubber which was attached to two -78° C. cold traps. At the end of the heating period, the remainder of the autoclave contents were slowly vented. The cold traps contained 36.1 g material which by GC analysis, contained 14.5% CF3CH2CF3 and 84.0% CF3CH2 CF2Cl, corresponding to a yield for CF3CH2CF2Cl of 69%. model autoclave fitted with a condenser was evacuated cooled to about -40° C. The temperature was increased to 120° C. maintained at that temperature for a total of 22 h was attached to two -78° C.