反应详情

温度

0 °C

Sodium hydride (60%, 326 mg, 8.14 mmol) was added to dimethyl sulfoxide (5 ml) under argon atmosphere and cooled to 0° C. To this mixture, diethyl 2-(7-octeny)malonate (2 g, 7.40 mmol) dissolved in dimethyl sulfoxide (5 ml) was slowly added, followed by stirring for 1 hour. After cooling to 0° C., 1-iodo-5,5,6,6,6-pentafluorohexane (2.68 g, 8.88 mmol) dissolved in dimethyl sulfoxide (5 ml) was slowly added to the reaction mixture, followed by stirring for 2 hours at room temperature. Water was added to the reaction mixture, which was then extracted with ethyl acetate. The organic layer was washed with water and dried over magnesium sulfate. After distilling off the solvent, the residue was purified by silica gel column chromatography (eluent: ethyl acetate/hexane=1/20) to give diethyl 2-(7-octenyl)-2-(5,5,6,6,6-pentafluorohexyl)malonate (2.3 g, Yield 70%) as a colorless oil.

1. additionwas slowly added
2. temperatureAfter cooling to 0° C.
3. additionwas slowly added to the reaction mixture
4. stirringby stirring for 2 hours at room temperature
5. extractionwas then extracted with ethyl acetate
6. washThe organic layer was washed with water
7. dry with materialdried over magnesium sulfate
8. distillationAfter distilling off the solvent
9. customthe residue was purified by silica gel column chromatography (eluent: ethyl acetate/hexane=1/20)