Organic Lab Reactions 69

Organic Lab Reactions 69 - 64 - ALIPHATIC FLUORINE...

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64 - ALIPHATIC FLUORINE COMPOUNDS mixture is poured into commercial hydrochloric acid while still hot 'and is washed free of antimony salt. The crude product, amounting to 910 g., solidifies at room temperature. By fractional distillation at 90 mm., it is separated into about equal parts of the monofluoride (b.p. 237°, m.p. 97°) and unchanged octachloropropane. » l,l,2,2,3,3-HexacMoro-l,3-difluoropropane (CCUFCC^CCUF). 80 In a round-bottomed flask equipped with an air-cooled reflux condenser a mixture of 1500 g. of octachloropropane, 560 g. of antimony, trifluoride, and 75 g. of antimony pentachloride is heated for five hours on a steam bath. A further quantity of 100 g. of antimony pentachloride is then added in small portions, and the heating is continued for twenty hours. The reaction mixture, which gradually becomes homogeneous, is al- lowed to cool before it is poured into aqueous acid, then is washed and dried. The crude product amounts to 1092 g., from which about 750 g. of difluoride is obtained by fractional distillation at 90 mm. The boiling
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