反応 #42130

反応方程式

chlorosulfuric acid

1,1,3,3,3-pentafluoropropene

→

CF3CH2CF2OSO2Cl

収率 72.7%

反応条件

後処理

1. 1
   温度cooled in liquid nitrogen
2. 2
   その他evacuated
3. 3
   温度to warm
4. 4
   workup.WAITAfter 24 hours
5. 5
   その他the reaction mixture quenched by ice
6. 6
   洗浄the organic layer washed with 5% sodium bicarbonate, water
7. 7
   その他dried under MgSO4
8. 8
   workup.DISTILLATIONAfter distillation

実験手順

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.

出典