Process for the preparation of perfluorinated cis-alkene
A cis-alkene, perfluorinated technology, applied in chemical instruments and methods, halogenated hydrocarbon preparation, organic chemistry, etc., can solve the problems of quinoline affecting results, undesired toxicity, etc.
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Embodiment 1
[0030] A 1 liter autoclave was charged with 2.0 g of catalyst (5% palladium on calcium carbonate, poisoned with 3.5% lead) and 160 mL of ethanol. The autoclave contents were then cooled to -78°C. Air was removed by pressurizing to 60 psi (434 kPa) with nitrogen followed by evacuation. This sequence is repeated two more times. Hexafluoro-2-butyne (32 g) was then added and the contents were heated to 25°C. Hydrogen was added to a pressure of 90 psig (651 kPa) and this pressure was maintained at a reaction temperature of 25-28°C for about 20 hours. The autoclave contents were cooled again with the aid of a -78°C bath before hydrogen evolution. The autoclave contents were distilled to obtain 31.6 g of 97% pure cis-hexafluoro-2-butene (97.5% yield). Three such preparations were performed and the combined material was redistilled to obtain the desired butene, bp 30-32° C., with a purity greater than 99.9% (H NMR: 6.56 ppm; F NMR: -60.17 ppm).
Embodiment 2
[0032] Example 2 was performed in a manner similar to Example 1, except that the ratio of hexafluoro-2-butyne to catalyst was doubled, and the hydrogen pressure was reduced to a maximum of 60 psig (434 kPa). Got similar results.
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Abstract
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