反应详情

温度

0 °C

To a solution of commercially available 2-trifluoromethylphenol (2.5 g, 15.42 mmol) in AcOH (3 mL) cooled to 0° C. was added dropwise concentrated HNO3 (1.5 mL). After the addition, the mixture was stirred at 0° C. for 5 min, at rt for 10 min, then poured into ice/water, and extracted with ether (3×). The combined ether extracts were washed with water, brine, dried (Na2SO4) and concentrated under reduced pressure. The residue was chromatographed (silica gel) eluting with 0% to 10% EtOAc/hexane to yield the title compound (1.4 g, 44% yield).

1. additionAfter the addition
2. extractionextracted with ether (3×)
3. washThe combined ether extracts were washed with water, brine
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated under reduced pressure
6. customThe residue was chromatographed (silica gel)
7. washeluting with 0% to 10% EtOAc/hexane