反应详情

A solution of 2-fluoro-5-nitroacetophenone (1.57 g, 8.6 mmol) in ethylene glycol (50 mL) was added hydrazine (0.29 g, 9.0 mmol) was stirred for 2 h at room temperature and then heated at 165° C. for 24 h. The reaction mixture was cooled to room temperature, poured over EtOAc (100 mL), and extracted with H2O (2×100 mL). The organic layers was dried over Na2SO4 and the solvent was removed in vacuo. The crude product was purified by silica gel chromatography to afford a light yellow solid (0.8 g, 53%) Rf=0.2 (EtOAc/hexane, 1/3). 1H NMR CDCl3 δ 8.63 (s, 1H), 8.23 (d, 2H, J=3 Hz), 7.46 (d, 1H, J=3 Hz), 2.60 (s, 3H).

1. temperatureheated at 165° C. for 24 h
2. temperatureThe reaction mixture was cooled to room temperature
3. extractionextracted with H2O (2×100 mL)
4. dry with materialThe organic layers was dried over Na2SO4
5. customthe solvent was removed in vacuo
6. customThe crude product was purified by silica gel chromatography