反应详情

On the other hand, to a solution of 3-oxo-dec-9-enoic acid ethyl ester (4.32 g, 20.3 mmol) in THF (15 ml) at 0° C. was added potassium tert-butoxide (2.73 g, 24.3 mmol) This resulting mixture was stirred at room temperature under nitrogen for 30 min. The mixture of 4,4,5,5,5-pentafluoro-iodopentane was added and mixture was refluxed under nitrogen for 2 days, and then poured into H2O. The mixture was extracted with hexane. The organic layer was washed with saturated aqueous NaCl, dried over Na2SO4, filtered, concentrated, and purified by column chromatography (silica gel, 60% CHCl3/hexane) to afford 3-oxo-2-(4,4,5,5,5-pentafluoropentyl)-dec-9-enoic acid ethyl ester (4.46 g, 59%).

1. additionwas added
2. temperaturemixture was refluxed under nitrogen for 2 days
3. extractionThe mixture was extracted with hexane
4. washThe organic layer was washed with saturated aqueous NaCl
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. custompurified by column chromatography (silica gel, 60% CHCl3/hexane)