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To a mixture of compound l-(6-chloro-5-methyl-3-pyridyl)ethanone (850 mg), compound l-(3,5- dichloro-phenyl)-2,2,2-trifluoro-ethanone (1.82 g) and K2C03 (862mg) in 20 ml of dichloroethane was added Et3N (50 mg). The mixture was refluxed for 16 h. After cooling to 0C, Bu4N+Br" (322 mg), NH2OH.HCl (690 mg, 10 mmol) and NaOH (800 mg, 4 N) was added and the reaction mixture was stirred at room temperature for 16 h. Then, the reaction mixture was poured into diluted hydrochloric acid and extracted with ethyl acetate three times. The combined organic layers were dried over MgS04 and concentrated under reduced pressure. The residue was purified by flash column chromatography on silica gel to give the title compound (1.6 g). lU NMR (300Mz, DMSO-d6): delta 2.39 (s, 3H), 4.37 (d, 1H), 4.43 (d, 1H), 7.62 (s, 2H), 7.83 (s, 1H), 8.17 (s, 1H), 8.55 (s, 1H).
With pyridinium chlorochromate; In dichloromethane; at 20℃; for 5h;
A mixture of PCC (4.26 g) and compound l-(6-chloro-5-methyl-3-pyridyl)ethanol (1.11 g) in 50 ml of DCM was stirred at room temperature for 5 h. Then the reaction mixture was filtered and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography on silica gel to the title compound (854 mg). lU NMR (300Mz, CDC13): delta 2.46 (s, 3H), 2.64 (s, 3H), 8.09 (s, 1H), 8.77 (s, 1H); ESI-MS: 170 (M + H+).
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