反应详情

Using essentially the same procedure as in Example 1, an isomeric mixture of the perfluorobutyric acid fluorides (2.67 g with summary acyl fluorides content 81%, 10 mmol), potassium fluoride (0.78 g, 13 mmol), the 1-methoxyheptafluoro-1-isobutene (5.10 g, 96% purity, 23 mmol) was combined in 8.54 g diglyme and agitated at room temperature for 34 hours. The reactor was vented and 5.44 g of material collected in the trap. The material consisted of (GC %): 4.0% starting C4 acyl fluoride, 35.3% C4F9OCH3, 58.5% hexafluoropivaloyl fluoride (C5 acid fluoride) and a trace (0.4%) of diglyme. To the diglyme residue was added 8.64 g H2O and 1.76 g triethylamine to yield 1.38 g CF3CH2CF3 (after recondensation), and 95.5 % purity. The products yields were calculated based on the weight of obtained mixtures, their GC % content and purity of starting compounds. Yield of C4F9OCH3 is 77% (from perfluorobutyric acid fluorides and 85% on the consumed fluorides). Yield of CF3CH2CF3 is 39% and C5 acid fluoride -65%.

1. custom5.44 g of material collected in the trap
2. additionTo the diglyme residue was added 8.64 g H2O and 1.76 g triethylamine