反应详情

Add n-butyllithium (1.6 M in hexanes, 4.9 mL, 7.8 mmol) dropwise over 5 min to a solution of 2,2,2-trifluoroethyl-p-toluene sulfonate (1.0 g, 3.9 mmol) in THF (20 mL) at −78° C. Stir for 30 min, add acetic acid (225 μL, 3.9 mmol) and stir for 30 min. Warm to room temperature, add ethyl acetate and extract with saturated aqueous ammonium chloride, and saturated aqueous sodium bicarbonate. Dry (magnesium sulfate), concentrate and purify (silica gel chromatography, eluting with 0:100 to 15:85 ethyl acetate:hexanes) to give the title compound as an oil (430 mg, 47%).

1. stirringstir for 30 min
2. extractionextract with saturated aqueous ammonium chloride, and saturated aqueous sodium bicarbonate
3. dry with materialDry (magnesium sulfate)
4. concentrationconcentrate
5. custompurify
6. wash(silica gel chromatography, eluting with 0:100 to 15:85 ethyl acetate:hexanes)