反应详情

In 20 ml of dichloromethane were dissolved 0.72 g of (S)-(-)-3-buten-2-ol (98%ee) and 0.95 g of pyridine, and then 1.65 g of 2,3,3,3-tetrafluoropropionyl chloride was dropwise added to the above-obtained solution while the solution was being cooled with ice. The resulting mixture was stirred at room temperature for 30 minutes, subsequently water was added thereto, and then the reaction mixture was subjected to extraction with ether. The resulting extract was washed with 1N hydrochloric acid, a 5% aqueous solution of sodium hydrogencarbonate, and brine, and then dried with magnesium sulfate. Subsequently, the solvent was removed under reduced pressure, and the residual product was distilled, thereby obtaining 1.50 g of 3-buten-2-yl 2,3,3,3-tetrafluoropropionate having the following physical properties.

1. temperaturewas being cooled with ice
2. extractionthe reaction mixture was subjected to extraction with ether
3. extractionThe resulting extract
4. washwas washed with 1N hydrochloric acid
5. dry with materiala 5% aqueous solution of sodium hydrogencarbonate, and brine, and then dried with magnesium sulfate
6. customSubsequently, the solvent was removed under reduced pressure
7. distillationthe residual product was distilled