反应详情

温度

55 °C

To a solution of (S)-5,6-difluoro-N-(1-(4-fluorophenyl)ethyl)-3-nitropyridin-2-amine (Method 53, 0.70 g, 2.3 mmol) in THF (12 ml) was added DIEA (0.39 g, 3.0 mmol) and 5-methyl-1H-pyrazol-3-amine (0.45 g, 4.7 mmol). The reaction was heated to 55° C. for 24 hours, cooled to room temperature, and quenched with water. The reaction was extracted with DCM (2×75 ml), and the combined organic fractions were dried over Na2SO4, filtered, and concentrated. The resulting oil was purified by column chromatography (DCM-MeOH=100:1) to give the title compound (0.60 g, 68%). MS: Calcd.: 374. Found: [M+H]+ 375.

1. temperaturecooled to room temperature
2. customquenched with water
3. extractionThe reaction was extracted with DCM (2×75 ml)
4. dry with materialthe combined organic fractions were dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe resulting oil was purified by column chromatography (DCM-MeOH=100:1)