反应详情

温度

80 °C

A mixture of (E)-1-(2-chlorobenzylidene)-2-(4-chloro-6-methylpyridin-2-yl)hydrazine (0.247 g, 0.882 mmol) and chloramine trihydrate (0.273 g, 0.970 mmol) in 7 mL of EtOH was heated at 80° C. for 2 h. After cooling to RT, water was added and the mixture was extracted with EtOAc (3×). The combined organic layers were dried over anhydrous sodium sulfate, filtered and concentrated to give 1.05 g of crude material. The crude material was purified by silica gel chromatography (50-75% EtOAc in hexanes) to afford 7-chloro-3-(2-chlorophenyl)-5-methyl-[1,2,4]triazolo[4,3-a]pyridine as an off white solid. MS (ESI, pos. ion) m/z: 278.0 (M+1).

1. temperatureAfter cooling to RT
2. extractionthe mixture was extracted with EtOAc (3×)
3. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. customto give 1.05 g of crude material
7. customThe crude material was purified by silica gel chromatography (50-75% EtOAc in hexanes)