反应详情

A 250 mL Hastelloy shaker tube was loaded with 60 g (0.51 mole) chlorosulfuric acid (HOSO2Cl), cooled in liquid nitrogen, evacuated and loaded with 60 g (0.45 mole) of 1,1,3,3,3-pentafluoropropene. The reaction vessel was allowed to warm and kept on a shaker at 20° C. at autogenous pressure for 24 hours. After 24 hours, the pressure tube was unloaded, and the reaction mixture quenched by ice and the organic layer washed with 5% sodium bicarbonate, water and dried under MgSO4. After distillation, 81.3 g of CF3CH2CF2OSO2Cl was obtained containing 6% of CF3CH2CF2OSO2F.

1. temperaturecooled in liquid nitrogen
2. customevacuated
3. temperatureto warm
4. waitAfter 24 hours
5. customthe reaction mixture quenched by ice
6. washthe organic layer washed with 5% sodium bicarbonate, water
7. customdried under MgSO4
8. distillationAfter distillation