反应详情

温度

70 °C

To a 30 ml toluene solution of 4-(2,2,2-trifluoroethoxy)phenol (1.02 g, 5.31 mmol) and diisobutylamine (0.074 ml, 0.42 mmol) was added sulfuryl chloride (0.38 ml, 4.7 mmol). This solution was heated to 70° C. for 2 hr. The solvent was removed under reduced pressure. The residue was diluted with AcOEt and sat. bicarb. solution. The organic layer was separated, and the aqueous layer was extracted twice with AcOEt. The combined organic layers were dried over anhydrous Na2SO4, filtered, concentrated, and chromatographed on silica gel eluting with 10% AcOEt/hexanes to give the title compound as a pale yellow oil 1.13 g (94%).

1. customThe solvent was removed under reduced pressure
2. additionThe residue was diluted with AcOEt and sat. bicarb
3. customThe organic layer was separated
4. extractionthe aqueous layer was extracted twice with AcOEt
5. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. customchromatographed on silica gel eluting with 10% AcOEt/hexanes