反应详情

温度

170 °C

To 2-fluorobenzophenone (1.0 g, 5.0 mmol) was added hydrazine (5 mL) and the reaction was heated to reflux for 3 hours. The reaction was then added to water (100 mL) and extracted with ethyl acetate (3×30 mL). The combined organic layers were dried with sodium sulfate (Na2SO4) and concentrated to an oil. The subsequent hydrazine adduct was heated with pyridine (20 mL) to 170° C. for 4 days. Pyridine was then removed under vacuum and the resulting oil taken up in water (100 mL) and extracted with ethyl acetate (3×30 mL). The combined ethyl acetate layers were dried (Na2SO4) and concentrated to give the final compound (650 μg, 67% yield). 1H NMR (CDCl3) δ 10.6 (br s, 1H), 8.04–7.99 (m, 2H), 7.56–7.50 (m, 2H), 7.47–7.33 (m, 2H), 7.29–7.19 (m, 3H); ES-MS (m/z) 195 [M]+.

1. temperaturethe reaction was heated
2. temperatureto reflux for 3 hours
3. extractionextracted with ethyl acetate (3×30 mL)
4. dry with materialThe combined organic layers were dried with sodium sulfate (Na2SO4)
5. concentrationconcentrated to an oil
6. customPyridine was then removed under vacuum
7. extractionextracted with ethyl acetate (3×30 mL)
8. dry with materialThe combined ethyl acetate layers were dried (Na2SO4)
9. concentrationconcentrated