反应详情

温度

60 °C

A three necked 500 ml reaction flask, equipped with a reflux condenser, a stirrer, a thermometer and a heating mantle was charged with 30.2 g of C4F9SO2F (0.1 moles), 15.1 g Na2SO3 (0.12 moles), 16.8 g NaHCO3 (0.2 moles), 50 g EtOH and 50 g DI-water. The reaction mixture was degassed 3 times using nitrogen and aspirator vacuum. The mixture was then heated to 60° C. under a nitrogen atmosphere for 16 hours. A slightly yellow reaction mixture with a pH of 6.5 was obtained. EtOH was stripped off under reduced pressure using an aspirator vacuum (20 torr and temperature between 60-85° C.) and the temperature was kept below 110° C. in order to avoid thermal decomposition of the sulfinate product. 19F analysis indicated a yield of 65% sodium perfluorobutyl sulfinate and 25% sodium perfluorobutyl sulfonate.

1. customA three necked 500 ml reaction flask
2. customequipped with a reflux condenser, a stirrer
3. customThe reaction mixture was degassed 3 times
4. customA slightly yellow reaction mixture with a pH of 6.5 was obtained
5. customan aspirator vacuum (20 torr and temperature between 60-85° C.)
6. customwas kept below 110° C. in order