反应详情

Trifluoromethanesulfonic anhydride (1.04 ml, 6.2 mmol) was added to a cooled (5° C.) solution of tert-butyl 4-hydroxybenzoate (1 g, 5.1 mmol) in a mixture of DCM (25 ml) and TEA (1.1 ml, 7.8 mmol). After 4 h at 5° C., water was added. The organic layer was separated, dried over MgSO4 and concentrated in vacuo. The residue was chromatographed over silica gel (eluent: cyclohexane/iPr2O 95/5) to yield the above-titled compound as a colorless oil (1.45 g). 1H NMR (CDCl3): 8.09 (2H, d, J=8.6 Hz), 7.32 (2H, d, J=8.6 Hz), 1.60 (9H, s).

1. customThe organic layer was separated
2. dry with materialdried over MgSO4
3. concentrationconcentrated in vacuo
4. customThe residue was chromatographed over silica gel (eluent: cyclohexane/iPr2O 95/5)