Sulfuric Acid → Tetrafluorosuccinyl fluoride
반응식
S(=O)(=O)(O)O.IC(F)(F)C(F)(F)C(F)(F)C(F)([F:12])I.[F:20][C:21]1([F:31])[C:26]([F:28])([F:27])[C:25]([F:30])(F)[O:24][C:22]1=[O:23]>>[F:27][C:26]([F:28])([C:21]([F:31])([F:20])[C:22]([F:12])=[O:23])[C:25]([F:30])=[O:24]참가 물질
4
반응 조건
- 온도
- 85 °C
실험 절차
Into a four necked flask equipped with a thermometer, a reflux condenser, a dropping funnel and a magnetic stirrer, 4950 g (18.5 moles as SO3) of fuming sulfuric acid containing 30% of SO3 were charged. The flask was heated to 85° C. and then, 990 g (2.2 moles) of 1,4-diiodoperfluorobutane having the forumla I (CF2)4I were added dropwise to the flask. The reaction was conducted for 6 hours while maintaining the temperature in the reactor at 85° to 95° C. The reaction mixture discharged from the reflux condenser, was passed through a gas washing bottle containing concentrated sulfuric acid and was collected in a flask cooled with a dryice-ethanol coolant. The collected reaction products in the flask were separated by distillation whereby 247 g of a fraction of a boiling point of 18° C. were obtained. According to F19NMR analysis of the fractions, the fraction having a boiling point of 18° C. consisted of 200g (yield of 47%) of perfluoro- γ-butyrolactone and 47 g (yield of 11%) of perfluorosuccinic difluoride. Another fraction having a boiling point of 1° C., 45 g (yield of 11% ) of perfluoroetrahydrofuran was also obtained.