反应详情

Triethylamine (25.83 ml, 185.3 mmol) and methanesulfonyl chloride (6.9 ml, 88.9 mmol) were added dropwise to a solution of 6,6,7,7,7-pentafluoroheptan-1-ol (14.1 g, 74.1 mmol) in dichloromethane (350 ml) at 0° C., followed by stirring for 1 hour. After the reaction was completed, water was added to the reaction mixture, which was then extracted twice with dichloromethane. The combined organic layers were washed with water and saturated aqueous sodium chloride, and then dried over anhydrous magnesium sulfate. After distilling off the solvent, the residue was purified by silica gel column chromatography (eluent: ethyl acetate/hexane=1/10) to give 1-methanesulfonyloxy-6,6,7,7,7-pentafluoroheptane (17.3 g, Yield 82%).

1. extractionwas then extracted twice with dichloromethane
2. washThe combined organic layers were washed with water and saturated aqueous sodium chloride
3. dry with materialdried over anhydrous magnesium sulfate
4. distillationAfter distilling off the solvent
5. customthe residue was purified by silica gel column chromatography (eluent: ethyl acetate/hexane=1/10)