反应详情

温度

50 °C

Sodium hydride (60% in mineral oil, 156 mg, 3.90 mmol) was added to a suspension of pyrazole (260 mg, 3.82 mmol) in N,N-dimethylformamide (5 mL) and the mixture was heated to 50° C. for 20 minutes. (4-Chloro-phenyl)-(6-chloro-pyrazin-2-yl)-carbamic acid tert-butyl ester (260 mg, 0.76 mmol) was added and stirring was continued for 30 minutes at the same temperature. The temperature was raised to 100° C. and the mixture was stirred overnight. The reaction mixture was quenched with brine and extracted with ethyl acetate (4×15 mL). The combined organic phases were washed with brine, dried over anhydrous sodium sulphate, filtrated and evaporated to give the crude product. Flash chromatography (ethyl acetate/heptane as eluent) gave (4-chloro-phenyl)-(6-pyrazol-1-yl-pyrazin-2-yl)-amine (56 mg, 27%) as a yellow solid.

1. temperatureThe temperature was raised to 100° C.
2. stirringthe mixture was stirred overnight
3. customThe reaction mixture was quenched with brine
4. extractionextracted with ethyl acetate (4×15 mL)
5. washThe combined organic phases were washed with brine
6. dry with materialdried over anhydrous sodium sulphate
7. filtrationfiltrated
8. customevaporated
9. customto give the crude product