反应详情

温度

25 °C

A solution of 2,3,5,6-tetrachloropyridine (0.20 g, 0.9 mmol), 5-cyclopropyl-1H-pyrazol-3-amine (0.20 g, 1.8 mmol), and triethylamine (0.10 g, 1.4 mmol) in NMP (2 ml) was heated in a microwave at 200° C. for 30 min. The reaction was cooled to 25° C., quenched with water (10 ml), and extracted with MTBE (4×30 ml). The combined organic fractions were then dried, filtered, and concentrated. The resulting solid was purified by column chromatography (DCM-MeOH=50:1) to give the title compound (0.035 g, 12%). MS: Calcd.: 303. Found: [M+H]+ 303.

1. customquenched with water (10 ml)
2. extractionextracted with MTBE (4×30 ml)
3. customThe combined organic fractions were then dried
4. filtrationfiltered
5. concentrationconcentrated
6. customThe resulting solid was purified by column chromatography (DCM-MeOH=50:1)