反应详情

温度

0 °C

2,2,3,3,3-pentafluoropropanol (3.0 g) was added to a suspension of sodium hydride (1.08 g) in dry ether (50 ml) at 0° C. under an argon atmosphere. Stirred at 0° C. for 15 minutes. Perfluoro-1-butanesulphonyl fluoride (12.08 g) was slowly added. Stirred at reflux for 3 hours, cooled and carefully quenched with H2O. Extracted with ether, twice. The combined extracts were washed with saturated brine dried over MgSO4, filtered and evaporated to give 2,2,3,3,3-pentafluoropropyl-1,1,2,2,3,3,4,4,4-nonafluorobutane-1-sulphonate as an oil. Yield 7.9 g. NMR: (CDCl3) δ 4.9 (m, 2H).

1. stirringStirred
2. temperatureat reflux for 3 hours
3. temperaturecooled
4. customcarefully quenched with H2O
5. extractionExtracted with ether
6. washThe combined extracts were washed with saturated brine
7. dry with materialdried over MgSO4
8. filtrationfiltered
9. customevaporated