反应详情

温度

50 °C

PPh3 (0.12 g, 0.45 mmol), Et3N (0.17 mL, 1.21 mmol), and CCl4 (0.044 mL, 0.45 mmol) were added to a stirred suspension of 4-(4-bromo-2-fluorophenylamino)-5-fluoro-1-methyl-6-oxo-1,6-dihydropyridine-3-carboxylic acid N′-(1-imino-ethyl)-hydrazide (0.073 g, 0.18 mmol) in methylene chloride (2 mL). The reaction mixture was stirred at 50° C. for 2 hours. After cooling to room temperature, the reaction mixture was diluted with ethyl acetate, washed with water, dried (MgSO4) and concentrated. Purification by flash column chromatography (4% MeOH in methylene chloride) gave clean desired product (30 mg, 50%); MS APCI (−) m/z 394, 396 (M−, Br pattern) detected; 1H NMR (400 MHz, CD3OD) δ 8.16 (s, 1H), 7.31 (dd, 1H), 7.25 (d, 1H), 7.01 (td, 1H), 3.67 (s, 3H), 2.51 (s, 3H).

1. temperatureAfter cooling to room temperature
2. washwashed with water
3. dry with materialdried (MgSO4)
4. concentrationconcentrated
5. customPurification by flash column chromatography (4% MeOH in methylene chloride)