反应详情

温度

28 °C

To a stirred solution of 2-chloro-5-fluorotoluene (0.500 g, 3.46 mmol, Lancaster, used as received) in conc. H2SO4 (5.0 mL) at 0° C., KNO3 (0.350 g, 3.46 mmol) was added in one lot. The resulting pale yellow solution was allowed to warm to 28° C. and stirred overnight at 28° C. It was then poured into ice (50 g) and extracted with ether (2×50 mL). The ether was dried over anhydrous Na2SO4, removed under vacuum, and the resulting oil was dried further under vacuum to afford 0.616 g (94%) of the title compound as an oil, which was used as such for the next reaction; 1H NMR (CDCl3): δ 2.459 (s, 3H), 7.193 (d, 1H, J1=11.1 Hz), 8.083 (d, 1H, J1=6.6 Hz).

1. extractionextracted with ether (2×50 mL)
2. dry with materialThe ether was dried over anhydrous Na2SO4
3. customremoved under vacuum
4. customthe resulting oil was dried further under vacuum