反应详情

Sodium hydride (325 mg, 8.12 mmol) was added to a solution of indazole (800 mg, 6.77 mmol) in N,N-dimethylformamide (10 mL) and stirred for 30 minutes. (4-Chloro-phenyl)-(6-fluoro-pyridin-2-yl)-amine (1.55 g, 6.77 mmol) was added and the reaction mixture was stirred at 80° C. overnight. The mixture was poured into a stirred ice-water solution and extracted with ethyl acetate. The combined organic phases were dried over magnesium sulphate, filtrated and concentrated in vacuo. The crude product was purified by column chromatography with ethyl acetate-heptane as eluent to give (4-chloro-phenyl)-(6-indazol-1-yl-pyridin-2-yl)-amine (230 mg, 11%) as an yellow solid. LC-ESI-HRMS of [M+H]+ shows 321.0901 Da. Calc. 321.090699 Da, dev. −1.9 ppm

1. stirringthe reaction mixture was stirred at 80° C. overnight
2. extractionextracted with ethyl acetate
3. dry with materialThe combined organic phases were dried over magnesium sulphate
4. filtrationfiltrated
5. concentrationconcentrated in vacuo
6. customThe crude product was purified by column chromatography with ethyl acetate-heptane as eluent