反应详情

To a stirred solution of 1-chloro-2,4-difluorobenzene (0.829 g, 5.58 mmol) in concd H2SO4 (8.0 mL) at 0° C., KNO3 (0.565 g, 5.59 mmol) was added in one portion. The resulting solution was allowed to warn to room temperature and stirred overnight at room temperature. It was then poured into ice (80 g) and extracted with ethyl acetate (75 mL). The ethyl acetate was dried over anhydrous Na2SO4, removed under vacuum, and the resulting oil was dried further under vacuum to afford 1.007 g (93%) pure (1H NMR) title compound as a light red oil; 1H NMR (CDCl3) δ 7.17 (dd, 1H, J1=9.9 Hz, J2=8.4 Hz), 8.24 (t, 1H, J=7.5 Hz).

1. customto warn to room temperature
2. extractionextracted with ethyl acetate (75 mL)
3. dry with materialThe ethyl acetate was dried over anhydrous Na2SO4
4. customremoved under vacuum
5. customthe resulting oil was dried further under vacuum